Cannabis testing

Customized solutions meeting latest regulations

Rookie of the Year

New benchtop instrumentMALDI-8020 complements the portfolio

Let’s have a party!

50th anniversary celebrationand future perspectives

Pharmaceutical

Plastics and Rubber

CONTENT

Clinical

Chemical, Petrochemical,Biofuel and Energy

The quantification of color – Study on color pigments with UV-Vis spectroscopy and coloranalysis software 2

Counting down the days –RoHS II – screening of phthal-ates in electrical and electronicequipment 6

Customized solutions for cannabis testing 8

Connecting wine to headaches –Determining higher alcohols andethyl acetate in wine 12

Run time cut, possibilities enhanced – Nexis GC-2030 quantifies contaminants in oil and gas for recycling 18

Acidic? Basic? Chelating? No problem for inert columns! –For reactive substances, inert LC columns are essential for a symmetrical peak shape 19

APPLICATION

Multimodal imaging by elemen-tal and molecular mass spectro-metry – Interview with Prof. Uwe Karst, University of Münster(Germany) 14

Let’s have a party! –50th anniversary celebration and future perspectives 22

LATEST NEWS

MARKETS

Rookie of the Year – MALDI-8020:new benchtop instrument in theMALDI portfolio 5

From fatberg to fuel – Controllingthe quality of biofuels with gaschromatography 16

PRODUCTS

SHIMADZU NEWS 3/2018

Food, Beverages, Agriculture

Environment

Automotive

The quantification of colorLaser toner and nail polish – Study on color pigmentswith UV-Vis spectroscopy and color analysis software

I nks and pigments make theworld colorful. But today,color is not purely ornamen-

tal, a signal or symbol, it can alsobe precious: toner for laser print-ers is said to be more expensivethan its weight in gold.

Depending on its characteristics,color generates films for protec-tion against sunlight, heat, corro-sion, and many more. To ensurea constant quality, color is pre-pared following regulations,which describe color scales tomake the production of colorindependent of human subjectivejudgement.

The material property “color” islinked to the absorption, trans-mission or reflection of visiblelight. Pigments absorb light ofsome wavelengths, appearing inthe complementary color to theabsorbed light. For this reason,UV-Vis spectroscopy is the toolof choice to measure the color ofpigments. While the wavelengthof transmission or reflectionmaxima already gives someimplication of the color, the useof color models independentfrom the measurement method ismuch more practical. With color

software, the transmittance orreflectance values are used for thecalculation of color coordinatesthat describe the color in thecontext of a given color model.

In this application, the ShimadzuUV-2600 spectrophotometerequipped with the ISR-2600plusintegrating sphere is used tomeasure diffuse reflection spectraof laser dye pigments and to cal-culate color coordinates of thesepigments with the LabSolutionsUV-Vis color software. Additio -nally, nail polish samples aremeasured in direct transmissionfor the color analysis.

Integrating spheres

The integrating sphere is a hol-low ball made of highly reflec-tive material with ports for de -tectors, samples or white stan-dards. Light entering the spherethrough an opaque solid or re -flecting into the sphere from a

Carbon content in ultrapure water – Risk assessment, experiments, measurements 11

READ FOR YOU

Figure 1: Shimadzu UV-2600

spectrophotometer

Figure 2: Shimadzu ISR-2600plus integrating sphere with beam diagram

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3SHIMADZU NEWS 3/2018

diffuse reflector will be collectedby the reflective inner surface ofthe sphere and recorded by thedetectors.

Figure 2 shows the schematic ofthe ISR-2600plus. The detectorsare mounted on top and bottomof the sphere and are excludedfrom the diagram on the rightside.

Sample and reference beam can beswitched depending on the targetmeasurement. To measure the dif-fuse only reflectance from a sam-ple, the sample is placed at port Cand the sample beam entersthrough port A. Specular reflected

light is excluded, as it exits thesphere through port A. To includespecular reflectance, the sample ismounted on port B and the sam-ple beam enters through port D.The incident angle of light to sam-ple surface in that case is 8 degreesand a mixture of specular and dif-fuse reflected light is included inthe measurement. For transmit-

tance measurements, the sample isplaced at port A. White standardsare used to close ports B and C ifno sample is placed there.

Color models

Two popular color models areused in this application. The colorvalues are calculated from thereflectance spectra by differentequations, that are not describedin detail here.

One color model is the tristimulusmodel [1], which describes coloras combination of three (abstract)color stimuli X, Y and Z. Thismodel is based on the three kindsof color receptors in human eyesand how the mixture of stimuli isinterpreted as color by our brain.

A graphical representation plotscolor coordinates x and y in a rep-resentation similar to the colorcircle (“color horseshoe”), asshown on the left side of figure 8(page 4).

The CIELab [2] model is based ona three-dimensional color spaceand was developed to representcolor in a manner that is consis-tent with human perception ofcolor. The axes of the three-dimensional coordinate system arebased on the three stimuli bright –dark, red – green and blue – yel-low.

Any point in the CIELab colorspace can be described by itslightness index L* and either incartesian color coordinates a* and

Figure 4: Laser dye film samples. From left to right: White, red and blue.

Figure 3: CIELab color scheme illustrated

as vectors

Figure 5: Nail polish film samples. From left to right: Gel blue, blue, turquoise, yellow, orange, pink, red.

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Blue Dye FilmRed Dye Film

Blue Dye PowderWhite Dye Powder

White Dye Film

200 300 400 500 600 700 800 900

Figure 6: Diffuse reflectance spectra of the laser dye samples Figure 7: Spectra of the nail polish samples. Inset: zoom into the spectra of the

turquoise and pink nail polish.

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Pink Nail PolishTurquise Nail PolishRed Nail Polish

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500 600 700 800

b* or in polar coordinates hueangle h° and chroma C*. Hue isthe color as in the color circle andchroma is the intensity of thatcolor. A graphical representationuses a two-dimensional plot forthe color coordinates at one fixedL* (right side of figure 8) or athree-dimensional color sphere.

Just as our perception of colorsdepends on the lighting condi-tions, the color values in eachmodel differ with the chosen ref-erence light source and observa-tion angle. This choice depends onthe purpose of the color measure-ment, e.g. color fastness of prod-ucts that are presented to custom -ers under defined lighting condi-tions. Here, the standard illumi-nant D65, �

Blue Laser Dye Film

Red Laser Dye Film

White Laser Dye Film

Blue Laser Dye Powder

White Laser Dye Powder

Blue Gel Nail Polish

Blue Nail Polish

Turquoise Nail Polish

Yellow Nail Polish

Orange Nail Polish

Pink Nail Polish

Red Nail Polish

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16.4

Sample Name Peak [nm] x y L* a* b*

that simulates sunlight, and anobservation angle of 10° wereused for all calculations.

Samples

Three powder samples and threefilm samples from ink and pig-ments were analyzed. The pow-ders were coarse and would be dif-ficult to measure by pressing intothe surface of Barium Sulphate(the preferred method of samplepreparation), so instead weremeasured in a special powder cell.Each of the laser dye samples wasmounted at the diffuse reflectanceport (port C in figure 2, page 2) ofthe integrating sphere. The refer-ence material was uncoveredBarium Sulphate, the surface mate-rial of the integrating sphere.

Seven different nail polishes wereapplied to glass substrates andmeasured with a film holder indirect transmission mode withoutintegrating sphere. A clean glassplate was used as reference.

Spectra

The diffuse reflectance spectra inthe range of 200 - 900 nm areshown in figure 4 (page 3). Thedark and light blue traces are fromthe blue dye film and powdermeasurements, the black and greylines are from the white dye filmand powder measurements and thered trace is from the red dye filmmeasurements.

this case and a more detailedanalysis is needed to discern itfrom the spectrum.

The spectra of the nail polish sam-ples are shown in figure 7 (page 3).

All film spectra show peak struc-tures in the range around 400 nm.These may be characteristic forthe film material or the base coatof the treatment. The spectra ofthe white samples show a more orless flat line over the visible range,as expected. The spectrum of thered sample shows a reflectancemaximum at 600 nm and generalhigh reflectance in the red spectralregion. The blue color is notreflected by specific peaks: bothfilm and powder sample of theblue dye show the highest reflec -tance in the region of 700 nm andabove and a small maximum at600 nm. Blue is a mixed color in

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4 SHIMADZU NEWS 3/2018

Most of the colors are alreadyindicated by the transmissionmaxima. The spectra of the bluenail polishes show a transmissionmaximum below 500 nm, at theedge of the blue and green spectralregion. Blue is again a mixed colorhere. The spectrum of the tur -quoise nail polish shows a trans-mission maximum around 500 nm,in the green spectral region. Thistransmission maximum is shiftedto longer wavelengths for theorange nail polish. The spectra ofthe yellow and red nail polishesdon’t show a sharp peak, but ageneral rise of the transmissionvalue that starts in the yellow andred spectral region, while the pinkline shows a steep rise of thetransmission value at 600 nm. All spectra show a rise of trans-mission towards the red end ofthe wavelength scale.

Color analysis

The five diffuse reflection spectrafrom figure 6 (page 3) and theseven transmission spectra fromfigure 7 (page 3) were evaluatedwith the LabSolutions UV-Viscolor module [3]. The evaluationtable is shown in table 1. Evalu -ation items are: peak wavelength,color coordinates x, y, a* and b*and lightness index L*. For allcolor coordinates and the light-ning index, standard illuminantD65 [4] was used as colorimetricilluminant and 2° as viewingangle.

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Blue Laser Dye Film

Red Laser Dye Film

White Laser Dye Film

Blue Laser Dye Powder

White Laser Dye Powder

Blue Gel Nail Polish

Blue Nail Polish

Turquoise Nail Polish

Yellow Nail Polish

Orange Nail Polish

Pink Nail Polish

Red Nail Polish

Figure 8: x-y-plot ( left side) and a*-b*-plot (right side) of the color coordinates from

table 1. Mind that brightness L* is not plotted, but it is different for all samples.

Table 1: Evaluation results for the dye UV-Vis measurements and the LabSolutions UV-Vis

color analysis.

Figure 8 shows the plot of the xand y color coordinates in the leftgraph and the plot of the a* andb* color coordinates in the rightgraph. This analysis shows, thatall expected colors are indeed

reflected in the color graphs, eventhough they might not be visibleat the first glance of the spectra.The white samples are placed inthe green region in the a*-b*-plotby their color coordinates, butthey show very high lightnessindices L*, near 100 %. All threevalues are important, when judg-ing a color. In the x-y-plot theyare at the white center, as expect-ed.

Conclusion

UV-Vis spectroscopy is a valuabletool for color analysis and qualitycontrol. Even though human indi-vidual perception of colors mightbe different, the use of color mod-els with defined illuminants andobservation angles allows to de -fine testable color coordinates.This analysis works well both fortransmission and reflection spec-tra. With the LabSolutions UV-Viscolor software, the color analysisis easily done without the need toexport data and it can even beautomated.

Special thanks to:Dr. Robert Keighley, Shimadzu UK for the

results of the laser dye measurements.

Literature[1] https://en.wikipedia.org/wiki/CIE_1931_

color_space

[2] https://en.wikipedia.org/wiki/CIELAB_

color_space

[3] ISO 11664-2:2007(E)/CIE S 014-2/E:

2006 colorimetric illuminants

[4] LabSolutions UV-Vis Brochure

PRODUCTS

5SHIMADZU NEWS 3/2018

Impressive performance

With a mass range of 1-500,000 Da,a mass resolution of more than5,000 (for ACTH18-39,m/z 2,465),a mass accuracy of < 20 ppm afterinternal calibration and a sensiti-vity of 250 amol (Glu-Fib, m/z 1,570), the MALDI-8020achieves the same specifications as the more advanced version, the Axima Assurance for highthrough put screening.

Compact size – quiet pumps

Thanks to its small dimensions of450 x 745 x 1,055 mm and weightof 86 kg, the new MALDI-8020fits on any lab workbench. Theoil-free diaphragm pump and aturbo pump ensure reliable andlow-noise operation (< 55 dB).

Optimized ion source for a faster analysis

Extra-fast motors drive the high-speed stage. Motor installationoutside the vacuum reduces thevolume to be evacuated, so pump-ing time after changing of sampleis the fastest on the market:around 90 seconds. The 200 Hzsolid-state laser allows furtheroptimization of the analysis time.The typical Shimadzu wide-bore

Rookie of the YearMALDI-8020: new benchtop instrument in the MALDI portfolio

T he new MALDI-8020 com-plements Shimadzu’sMALDI family. The linear

benchtop time-of-flight massspectrometer serves various appli-cations in the positive ion mode,such as analysis of proteins, pep-tides or polymers. It is ideal forresearchers developing MALDI-based diagnostic methods, and forroutine labs carrying out qualitycontrol and fast analysis of intactsamples.

The MALDI-8020 is fast andaccurate, has a high resolution andits compact size makes it fit in anylaboratory. The robust designpromises reliable analysis and lowmaintenance. The MALDI-8020’sfeatures make it the ‘Rookie of theYear.’

Rookie of the year: the new compact MALDI-8020

ion optics increase ion transmis-sion and reduce the likelihood ofcontamination. If the source isnevertheless contaminated, it canbe cleaned within ten minutesusing the UV laser-basedTrueClean.

Various fields of application

The MALDI Solutions softwareprovides intuitive and easy opera-tion, and includes interfaces forevaluating polymer, protein andoligonucleotide spectra.

SampleStation, AuraSolution andQC Reporter offer various op -tions for automated lab routines.During sample preparation, data can be collected with theSampleStation software.

The barcode reader integrated intothe mass spectrometer enablesautomated measurement usingAuraSolution. The QC Reportersoftware allows specification ofdifferent criteria that can be usedfor automatic evaluation of theanalyses.

Data is stored in a Microsoft®

SQL database with automaticbackup. Personalized user loginscan be used to document qualitycontrol, and different levels can beassigned to individual users. Inthis way the user is prepared forpotential audits.

Conclusion

The MALDI-8020has a compact androbust design andoffers a low-costsolution for broadfields of applica-tion, includingresearch and teach-ing as well as quali-ty control.

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PublisherShimadzu Europa GmbHAlbert-Hahn-Str. 6 -10 · D-47269 DuisburgPhone: +49 - 203 - 76 87-0 Fax: +49 - 203 - 76 66 25shimadzu@shimadzu.euwww.shimadzu.eu

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CopyrightShimadzu Europa GmbH, Duisburg, Germany – November 2018.

Windows is a trademark of Microsoft Corporation. ©2018

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6 SHIMADZU NEWS 3/2018

O n 22nd of July 2019, the EU RoHS II directive willcome into effect. The tran-

sition period will then be over andlimit values for four phthalic acidesters in electrical and electronicequipment must be adhered to.

Some phthalic acid esters, knownas phthalates, have been banned inEurope since years due to theirpotential health risks. Since 2009,limit values have been applied tothe content of certain phthalatesin toys and baby products whichcan be hazardous when put intochildren’s mouths. The list ofproducts for which phthalate con-centration is regulated by law isexpanding constantly. It coverscosmetics, plastics for food pack-aging and soon also electrical andelectronic equipment.

Time and again, some phthalatesmake headline news as substanceshazardous to health. Low molecu-lar phthalates such as di-(2-ethyl-hexyl)-phthalate (DEHP), dibutylphthalate (DBP), benzyl butylphthalate (BBP) and diisobutylphthalate (DIBP) are especiallysuspected of having an endocrino-logical (hormone-like) effect.Endocrine disruptors affect hor-monal balance and can causehealth disorders in sufficientlyhigh concentrations. The effect ofsubstances that interfere with thesex hormone system and impairreproductive ability is currentlythe subject of heated debate.

DEHP, BBP, DBP and DIBP in the RoHS II Directive

The compounds listed above(DEHP, BBP, DBP and DIBP)have therefore been included inthe EU REACH chemicals regula-tion. Since February 21 2015, theymay only be produced and usedwith a special exemption that isdifficult to obtain. Additionally,the European Commission hasdecided to restrict the four phtha-

lates with the RoHS II Directive(Directive on the restriction of theuse of certain hazardous substanc -es in electrical and electronicequipment).

The RoHS II Directive specifies a maximum permissible concen-tration of 0.1 mass percent (i.e. amaximum of 1,000 mg/kg) persubstance. The planned transitionperiod expires for most devicegroups on 07/22/2019. Medicaldevices as well as control andmeasuring instruments have alonger period until 2021.

Phthalates are still used world-wide as plasticizers, especially inplastics such as PVC, nitrocellu-

Counting down the daysRoHS II – screening of phthalates in electrical and electronic equipment

lose or synthetic rubber. Accord -ing to current EU legislation,manufacturers of electrical andelectronic equipment are nowobliged to ensure that their equip-ment complies with RoHS. Themanufacturers must thereforeensure that the content of the fourregulated phthalates is lower thanthe limit of 1,000 mg/kg. In par-ticular, companies that processsupplied products must rely onthe supplier or check for them-selves.

Special screening method forphthalates in polymers

The IEC 62321 international teststandards provide methods

enabling the electrical industry todetermine the concentration ofcertain regulated substances inelectrical products on a globallyuniform basis. Part 8 of this stan-dard (IEC 62321-8:2017) describesthe method for determination of“phthalates in polymers by gaschromatography mass spectrome-try (GC-MS) and gas chromatog-raphy mass spectrometry usingthe addition of pyrolysis/thermaldesorption (Py/TD-GC-MS).“The Py-Screener described herewas specially developed as ascreening method to determinephthalates in polymers and is fullycompliant with Part 8 of the IEC62321 standard.

A major advantage of this screen-ing method: it needs very littlesample preparation, and the com-plete method package allows poly-mer samples to be analyzed quick-ly without the necessity for extramethod development. Classicalmethods of analyzing and quanti-fying phthalates are based oncomplex sample preparation. Inthis case, extraction of the samplesoccurs using a solvent over severalhours, with subsequent GC-MSanalysis.

The Py-Screener is based on acoupled pyrolysis GC-MS. Formeasurement, a small piece of thepolymer sample (approx. 0.5 mg)is placed in a stainless steel cupand entered in the preheatedpyrolysis furnace using an auto -sampler. The semi-volatile phtha-lates are extracted from the poly-mer using a special temperatureprogram. Gaseous phthalates aretransported with a helium carriergas stream into the gas chromato-graph, separated on the analyticalcolumn and then identified andquantified with the mass spectro -meter.

Pyrolysis GC-MS method package

The method package of the Py-Screener supports users right fromthe beginning with a detailed man-ual describing each step. Samplepreparation of standards and poly -mer samples can even be followedvia a video tutorial. Depending onthe shape, the sample is punchedout or cut with the tools from thetoolkit (figure 2) and then weighed

Figure 1: Pyrolysis-GCMS

Figure 2: Sample preparation tool kit

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7SHIMADZU NEWS 3/2018

for quantification. Method andinstrument parameters are alreadyoptimized for the analysis ofphthalates; batch tables for sam-pler and instrument software onlyhave to be filled in.

Calibration and quantificationparameters are already part of themethod, including QA/QC con-trols to check sensitivity of thesystem and column performance.With the unique AART function(Automatic Adjustment of Reten -tion Time) of the GCMSsolutionsoftware and a simple alkane stan-dard, retention times of the quan-tification table can be adapted eas-ily and quickly to a new columnor, after maintenance work, to theshortened column.

Measurements are evaluated in theLabSolution Insight software,which was developed specially forprocessing large sample quantities.Data is presented clearly in tabu-lar and graphical form, and thequantification results are color-coded with so-called flags (figure3). This allows users to see with aglance whether the concentrationof a polymer sample is harmless orfar above the limit value. In bothcases, the sample requires no fur-ther analysis.

Screening and exact quanti-fication without modificationusing GC-MS

However, if the phthalate concen-tration determined by the screen-ing method is within the range ofthe limit value (500 -1,500 mg/kg),a second, more precise quantifica-

tion should be carried out to deter -mine the exact concentration. Onepossibility is the classical GC-MSmethod with prior extraction ofthe sample and subsequent liquidinjection.

Shimadzu’s Twin Line MS Systemis an ideal solution. It is equippedwith an additional liquid injector,an autosampler (AOC-20i) and asecond capillary column. With aspecial kit, both columns can beinstalled simultaneously in themass spectrometer as the powerfulturbomolecular pump of theGCMS-QP2020NX allows a col-umn flow of up to 15 mL/sec.With this system, ei ther polymersamples can be screened or extract -ed liquid samples can be quantifiedexactly with out further modifica-tion of the GC-MS.

The all-round package alsoincludes a “Maintenance Navi -gator“ which supports users withdetailed descriptions and clearstep-by-step illustrations for regu-lar maintenance work, such asreplacing the pyrolysis or injectorliner. If a leak occurs in the sys-tem, the “Maintenance Navigator“provides valuable information forsystematic troubleshooting (fig-ures 4a and 4b).

Analysis of polybrominatedflame retardants

In addition to limit values forsome heavy metals, the RoHS IDirective already prescribes amaximum concentration for theorganic compounds PBB (poly-brominated biphenyls) and PBDE

(polybrominated diphenyl ethers)used as flame retardants. Thesecompounds are also GC-MS com-patible and can be analyzed withthe Py-Screener system. The opti-mized methods are already part of the package and can be useddirectly if required.

Conclusion

The “Py-Screener“ screening sys-tem is a comprehensive packagefor the analysis of phthalic acidesters in electrical products and iscompliant with Part 8 of the IEC62321 standard. The package con-tains optimized method andinstrument parameters, ready-made sequences for pyrolyzer andGC-MS software, a toolkit forsample preparation and specialevaluation software. This makesquantification of phthalates easyto learn, even for new users. As ascreening method, the Py-Screenersaves both solvent consumptionwhen compared to classical meth-ods, and time, since many poly-mer samples can already be ex -cluded from further analysis afterthe first measurement.

Literature[1] Official Journal of the European Union

6/4/2015.

[2] Commission Delegated Directive (EU)

2015/836 of 31st of March, 2015,

directive of the European Parliament

and of the Council amending Annex II

to Directive 2011/65/EU as regards

the list of substances subject to restric-

tions.

Figure 3: Special evaluation software: For faster optical identification, different

concentrations of indicator substances are highlighted in color.

Figures 4a and 4b: Examples from the

Maintenance Navigator

Further information

on this article:

• Brochure: C146-E285

Py-Screener

• Application: Analysis

of Phthalate Esters using the Py-

Screener (1) (LAAN-J-MS-E110);

Analysis of Phthalate Esters using the

Py-Screener (2) (LAAN-J-MS-E111)

• Technical Report: Comparison of

Screening Method (Py-GCMS) and

Quantitative Method (Solvent Extrac -

tion-GCMS) for Phthalate Ester Analysis

APPLICATION

8 SHIMADZU NEWS 3/2018

A s of July 2018, over 20Euro pean countries havelegalized cannabis for medi -

cal use, and more are expected tofollow in the coming years. Pos -session of cannabis is still illegalby federal statute; however thereis an ongoing debate concerninglegalization of medical and recre-ational cannabis. The demand forcannabis testing and analyticaltools is therefore growing.

Numerous health benefits havebeen reported for cannabis, includ -ing general pain reduction, anti-nausea and reduction of seizuresand autism. QC testing for can -nabinoids is essential for the accu-rate labeling of cannabis productsin both medical and recreationalcannabis markets. Cannabinoidsare the primary active componentsof cannabis; these are target com-pounds for potency testing. Ter -penes influence the homeopathiceffect, and contaminants such aspesticide residues and mycotoxinein cannabis products also need tobe controlled to ensure consumersafety.

Shimadzu offers a wide range ofanalytical equipment and providescustomized solutions, appropriateconfigurations and applicationsupport for cannabis analysis,including sample preparation.

Potency testing for cannabisproducts by HPLC

While the reason for controversyof cannabis as a legal medicine isthe psychoactive effect of onlyone of the cannabinoids con-tained, namely �9-tetrahydro-cannabinol (d9-THC), therapeuticbenefits such as pain relief andreduced severity of nausea andseizures were also reported withuse of a combination of otherphytocannabinoids [1, 2]. Addi -tionally, a number of studies

no or neglectable d9-THC con-tent are therefore becomingincreasingly popular, as they can

another major component of can -nabis, has so far been demonstrat-ed [3, 4]. CBD-rich products with

showed high safety with regard toa wide array of side effects and notolerance to cannabidiol (CBD),

Customized solutions for cannabis testingAnalytical solutions meeting latest regulations

Figure 1: Cannabinoids determined in potency testing

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Minutes Minutes

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Figure 2: Representative chromatograms for total cannabinoid content (a + c) and CBD content (b + d) in two different hemp oils

9SHIMADZU NEWS 3/2018

APPLICATION

be obtained legally without theprescription necessary for d9-THC containing medication.

Regulatory demands regardingd9-THC make it the primaryfocus of potency testing. Cannabisplant material contains d9-tetra -hydrocannabinolic acid (THCA),the non-psychoactive, carboxylicacid form of d9-THC which is theprecursor and is converted toTHC upon heating. High per-formance liquid chromatography(HPLC) is the method of choicefor quantification of cannabinoidsin the presence of their acid form,as the high temperatures in gaschromatography (GC) only allowdetermination of total THC.

Cannabis “potency” is normallydetermined by quantitation of themajor cannabinoids, includingTHCA, THC, CBD and CBN.The i-series HPLC analyzer forpotency testing of cannabis prod-ucts enables reliable quantificationof eleven important cannabinoids(figure 1) using a fast and simpleHPLC-UV assay. In the exampledescribed it was used for qualitycontrol in hemp oil with regardsto the label claim of CBD as wellas THC content.

Five hemp oil samples from vari-ous mail-order vendors were dis-solved in isopropyl alcohol, dilut-ed with methanol and filteredprior to HPLC analysis. Figure 2

shows chromatograms obtainedfrom analysis of two differenthemp oil samples for determina-tion of total cannabinoid content(81 x diluted) as well as CBD con-tent only (405 x dilution).

Two of the five oils tested wereclear with a weak yellow/greencoloration and showed high ratiosof CBD to total cannabinoid con-tent (92 %). Both samples alsotested close to label claim at 95 %and 92 % respectively. This led tothe assumption that each of theseoils was a product of multi-steppurification after extraction.

A third sample on the other handwas not transparent, and brown/

green and gritty in appearance. It also exhibited a distinctly“earthy” odor and revealed thehighest content of CBD and totalcannabinoids, with the lowestratio of CBD to total cannabi-noids (59 %). It was most likelythe result of crude extraction only,with no further refinement.Although its CBD % of labelclaim tested the lowest (81 %),this sample contained the highestlevel of CDB compared to allother oils tested.

The two remaining hemp oils tested higher than label claim at122 % and 200 % respectively,calling into question the type andaccuracy of testing used to justifylabel claim.

All samples contained less than 0.3 % d9-THC, as expected fromhemp products. This study showedthat in three out of five randomlyselected samples the actual con-centration of CBD did not com-ply with the stated content, andprovides a simple and fast assayfor CBD and total can nabinoidcontent for improved quality con-trol of cannabis products.

Terpene profiling by GC-MS

Terpenes and terpenoid com-pounds are produced in tri -chromes (where THC is generat-ed) and give cannabis its uniqueflavor and fragrance. Aside fromtheir aromatic properties, terpenesalso have advantageous healthbenefits. They act as essential,medicinal hydrocarbon buildingblocks and have a synergistic rela-tionship with cannabinoids, influ-encing the overall homeopathiceffect. �

Figure 3: TIC chromatogram of terpene standard

1.02.03.04.05.06.07.0

(x 100,000)

6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0

00.050.1

0.150.2

0.250.3

0.350.4

0.450.5

Wt % of Terpenes in Cannabis

Figure 4: Terpene distribution in three different strains of cannabis: CB Diesel, Blue Dream and Haze Wreck

APPLICATION

From the pine odor of pinene tothe citrus-like smell of limonene,characterization of terpenes isachieved easily using gas chro-matography. With the ShimadzuGCMS-QP2020, HS-20 headspace sampler and NIST spectrallibrary more than 3,000 flavor andfragrance compounds can be iden-tified for most efficient terpeneprofiling.

Cannabis has over 140 terpenecomponents, many of which areof medicinal interest [5]. Predomi -nant terpenes in cannabis include • �-myrcene, which has antibioticproperties and enhances theTHC muscle relaxant effect, • �-pinene, which improves theTHC bronchodilator effect andexhibits anti-inflammatoryproperties and • �-caryophyllene, which also actsas an anti-inflammatory agentand increases the THC gastriccytoprotective effect, amongstother health benefits [6, 7 ].

The concentration of individualterpenes varies by strain, can beanywhere from 0.1 to 1.5 % of itstotal dry weight and can varydepending on harvest time, dryingand storage conditions. Terpenelevels can decrease over time andcan, after three months of storage,be reduced by more than half [8].

The decrease in terpene amountover time varies for different ter-penes. Due to the uniqueness ofterpene profiles, they can be usedby cultivators as a “fingerprint” to partially ID the specific strainin question. As an example, theanalysis of several strains ofcannabis for 41 terpenes usingGC-MS with headspace injectionis described here.

A five-point calibration curve wascreated with concentrations rang-ing from 12.5 - 100 µg/mL. A partof the flower weighing 1.0 gram

ten to one and RSD of 20 % orbetter were required at the limit of quantitation. In addition,reproducibility of three QC repli-cates in three different cannabisstrains was also required to bewithin 20 % RSD.

The most commonly detected pes-ticide was piperonyl butoxidewhich finds wide use in pesticideformulations to enhance activityof the main ingredient. It wasdetected over a wide range of con-centrations. Myclobutanil, an anti-fungal known to be used in can -nabis cultivation, was detected ina number of samples as well.Among the cannabis concentrates,a high percentage tested positivefor one or more pesticides.

Literature[1] Perry G. Fine, Mark J. Rosenfeld,

Rambam Maimonides Medical Journal,

October 2013, Volume 4, Issue 4.

[2] Klein TW, Newton CA, Adv Exp Med

Biol. 2007;601:395-413.

[3] LM Borgely, et al., “The pharmacologic

and clinical effects of medical

cannabis”, Pharmacote-herapy (Review)

33 (2):195-209 (February 2013).

[4] Kerstin Iffland, Franjo Grotenhermen

Cannabis and Cannabinoid Research

Volume 2.1, 2017 DOI: 10.1089/can.

2016.0034.

[5] Giese, M.W., Lewis, M.A., Giese, L. and

Smith, K.M. Development and Valida -

tion of a Reliable and Robust Method

for the Analysis of Cannabinoids and

Terpenes in Cannabis. Napro Research,

California, 2015.

[6] Parland, J.M., and Russo, E.B. Cannabis

and Cannabis Extracts: Greater than the

Sum of Their Parts? The Haworth Press,

Pennsylvania, 2001.

[7] E. Russo, Taming THC: Potential Canna -

bis Synergy and Phytocannabinoid-

Terpenoid Entourage Effects, British

Journal of Pharmacology 163 (2011)

1344.

[8] Chemistry and Analysis of Phytocanna -

binoids and Other Cannabis Constitu -

ents. Humana Press, New Jersey.

Shimadzu does not support or promote

the use of its products or services in con-

nection with illegal use, cultivation or

trade of cannabis products. Shimadzu is

not condoning the use of recreational nor

medical marijuana, we are merely provid-

ing a market summary of the cannabis

testing industry.

https://www.shimadzu.eu/cannabis-testing-

solutions

tive detection of chemical residuecontamination is necessary forconsumer protection. QuEChERSextraction and LC-MS analysisoffer effective and efficient detec-tion of pesticides commonlyemployed during cannabis cultiva-tion.

Pesticide-free organically-growncannabis was used for spikingstudies and calibration curves. A variety of cannabis samplesoffered for retail sale, includingcannabis concentrates, were thenanalyzed for pesticides.

Samples were prepared accordingto the QuEChERS extraction pro-tocol (figure 5) and analyzed usinga Shimadzu Prominence HPLCwith LCMS-8050 triple quadru-pole mass spectrometer. Electro -spray ionization in continuouspolarity switching mode was usedfor detection.

Optimized MRM settings wereused for each compound and atleast one quantifier and one quali-fier transition were selected. Theretention times were determinedand used to program the MRMsegments for optimum duty cycle.Figure 6 shows a representativechromatogram of pesticide mixspiked in cannabis matrix at anintermediate level (31 ppb).

The calibration curve was pre-pared in spiked matrix over therange of 20 to 2,000 ng/g driedflower weight. Limits of quantita-tion were determined by measur-ing samples in triplicate at variouslevels. Signal-to-noise of at least

was frozen, followed by grindingto ensure a representative sample.Ten to 30 mg of the flower werethen weighed into a headspace vialand capped. The final result wascalculated to give wt %.

The first sample of cannabis, CBDiesel, was analyzed shortly afterharvest. The resulting wt % ofterpenes was similar to that incurrent literature [5]. The twoother samples, Blue Dream andHaze Wreck, were stored at ambi-ent temperature and exposed tolight for one month prior toanaly sis. It has been demonstratedthat different storage conditionscan change terpene results overtime, which should be taken intoconsideration when analyzingcannabis samples (figure 4, page 9).

Pesticide screening by LC-MS-MS

Pesticides are used in commercialcannabis grow operations to killinsects and spiders that thrive oncannabis plants. Above certainlevels pesticides may be carcino-genic and mutagenic, causing seri-ous harm to consumers, especiallyimmuno-compromised medicinalcannabis users. Sensitive and selec -

10 SHIMADZU NEWS 3/2018

Figure 5: QuEChERS extraction of dried cannabis flower

for pesticide analysis

(x 100,000)

0.00.10.20.30.40.50.60.70.80.91.01.11.21.21.41.5

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Figure 6: Representative chromatogram of pesticide mix spiked in cannabis matrix

READ FOR YOU

11SHIMADZU NEWS 3/2018

M any industry sectors suchas pharmaceutical pro-duction or semiconduc-

tor manufacturing require ultra-pure water. Regular controls ofthe organic carbon content arenecessary to make sure the waterquality complies with specifica-tions.

The definition of the purity ofultrapure water for production isbased on various physical, chemi-cal and microbiological parame-ters. A central sum parameter isthe content of total organic car-bon (TOC). It comprises thelargest of all substance groups.

To determine TOC, the ultrapurewater sample is mixed with anacid which converts the inorganiccarbon compounds, carbonatesand hydrogen carbonates, intocarbon dioxide. A purge gas, usu-ally synthetic air, expels theresulting CO2. An aliquot of thesample is then oxidized to convertthe dissolved organic substancesto carbon dioxide, which is detect-ed by a non-dispersive infrared(NDIR) detector.

Regular inspection

No matter how ultrapure water isproduced, it is never completelyfree of foreign substances such asorganic compounds. Over time,carbon content in the waterincreases. Materials in contactwith water release organic sub-stances, and organic and inorganicsubstances are dissolved from theambient air into the ultrapurewater. It is therefore challengingto store and handle ultrapurewater, and it must be checkedbefore use. In TOC analysis,ultrapure water is both sampleand operating material; it is con-tained in the rinsing solutions ofthe analyzers and used to preparecalibration solutions.

Due to the blank value or residualconcentrations of the ultrapurewater used in standard solutions,the results shift to higher meas-ured values, and the calibrationcurve therefore gets a positive Y-axis section. The smaller themeasuring range, the greater theinfluence of the blank value on thecalibration.

For TOC measurement of ultra-pure water samples and samples inthe trace range, a positive Y-axissection is not desirable, since suchsamples do not have residual con-centrations. Using the calibrationcurve for quantification with theformula: TOC content = (mea-sured area value minus axis inter-cept) divided by the slope, theTOC content would be changedunintentionally. To avoid this, azero offset, the parallel shift of thecalibration line through the zeropoint is necessary. It needs to beperformed ahead of evaluation inorder to subtract the blank valuefrom the preparation of the stan-dard solutions with TOC content(figure 1).

Impurities from the environment

In addition to blank values fromthe ultrapure water and the re -

agents used, impurities from theenvironment can also be presentin the TOC measurement. Theseare often random, and in manycases neither reproducible norclearly determinable. For example,they originate from residues insample bottles, measuring vesselsand chemicals, or from the labora-tory environment.

To illustrate this contaminationprocess, ultrapure water from abottle (HPLC ultrapure water)was analyzed. TOC specificationof the water was below 5 µg/L.An aliquot of the sample wastaken, analyzed, and the bottleclosed tightly. Even the firstanalysis value did not meet thespecifications as it showed a high-er TOC content of 25 µg/L. Thisexamination was repeated severaltimes within three hours. Duringthis period, the TOC contentincreased to over three times theinitial value (table 1, page 12).

The type and number of sourcesof contamination, their influenceand effect on trace analysis de -pends among other things on thestructure, equipment and analyti-cal parameters of a laboratory. It is therefore necessary for everylab doing ultrapure water meas-urements to identify sources of

contamination and to evaluatethem through tests and examina-tions of the lab processes. On thebasis of a risk assessment, meas-ures must be taken to limit thecarbon input to an acceptablelevel.

Identifying contaminationsources

A simple experiment shows howlarge the TOC input from the laboratory air can be. Four bea -kers, 100 mL each, remained opento the environment of the TOClaboratory. The ultrapure waterfrom a fifth beaker was filleddirectly and acidified for themeasurement. Every two hours,one of the four open beakers wasfilled and acidified for analysis. In the end, all five samples (0 h, 2 h, 4 h, 6 h and 8 h) were testedfor TOC.

In addition to laboratory space, itmay be useful to examine adjacentareas or the outside air to findcontamination paths. This testsetup works analogously withoutacidification for conductive inor-ganic and organic compounds.

Another useful test, even if all laboratory processes work well, is to check the glassware set forTOC entry. At random, at leasttwo of each of the glassware fromthe laboratory cabinet would beremoved for TOC analysis. Onefrom each pair is then prewashedaccording to the working instruc-tions. The other glassware is usedwithout further preparation. Forthe actual test, the glass vessels arefilled with ultrapure water withknown TOC content (blank valuemeasurement) and left to sit for atleast two hours before samples aretaken. In case of small glasswaresuch as 10 mL volumetric flasks,several can be flushed.

For sample vessels or storage con-tainers for acids, standards orrinsing solutions, it makes senseto extend the time span usuallyused for sampling or analysis. Theuse of plastic vessels is not recom-mended for TOC trace analysis.But if they are already in use,glass and plastic should then becompared. �

Carbon content in ultrapure waterRisk assessment, experiments, measurements

0

10

20

30

42.0145

0 0.5 1 1.1

Concentration [mg/L]

Area

Figure 1: Calibration function with zero offset at TOC-LCPH

APPLICATION

T he taste and aroma of winesrelate to the amount of different alcohols and sol-

vents like methanol, butanol andethyl acetate. These are said to bethe main reasons for causing

isoamyl alcohol and metha nol [1, 2].

Winemakers are therefore interest-ed in a quantification of these sub-stances. Controlling fermentation

give a solvent-like taste. Duringfermentation, yeast makes aceticacid and ethanol react to form the pleasantly tasting ethyl ace -tate, but also generates the un -comfortable alcohols isobutanol,

head aches, next to dehydration,histamines (see Shimadzu-NEWS3/2005), sulfites and tannin.

While ethyl acetate as an esterbrings a fruity taste, the alcohols

Connecting wine to headachesDetermining higher alcohols and ethyl acetate in wine

READ FOR YOU

Conclusion

It is easy to carry out tests to seehow far organic substances con-taminate ultrapure water. The testsindicate the extent to which theenvironment affects the contami-nation of ultrapure water. Hence,it is possible to observe and re -duce the carbon input.

This article was written in cooper-ation with Mr. Arno Bayerl,Divisional Head cleaning valida-tion and hygiene, TECHPharmGmbH.

Read for you in Nachrichten aus derChemie 5/18

12 SHIMADZU NEWS 3/2018

Table 1: Table of test results

1

2

3

4

5

6

12 :08

13 : 01

13: 25

14: 14

14: 40

15:10

25.21

34.08

35.77

55.88

75.08

79.25

4

4

4

4

4

4

Withdrawal Time NPOC in µg/LInjections per

sample

Methanol

n-Propanol

Ethyl acetate

2-Butanol (ISTD)

Isobutanol

Isoamylalcohol

170

34

68

100

41

241

28

39

58

100

24

120

Compound Red wine [mg/L] Shimadzu wine [mg/L]

Injection volume

Injector temperature

Carrier gas

Carrier gas speed

Column oven program

FID temperature

Parameter1 µL, Split 1 : 10

220 °C

He

30 cm/s, linear velocity mode

40 °C, 3 min, 5 °C/min, 50 °C, 4 min, 5 °C/min, 70 °C,

3 min, 45 °C/min, 240 °C, 5 min

260 °C

Value

13SHIMADZU NEWS 3/2018

APPLICATION

for better taste, and even moreimportantly reducing damage tohealth by alcohols other thandrinking alcohol, are main con-cerns.

Higher alcohols in wine with GC-FID

Determining higher alcohols withthe GC-2030 gas chromatographand a flame ionisation detector(FID) is a fast and efficient way to measure the amount of ethylacetate, isoamyl alcohol, n-propa -

nol, isobutanol and even metha -nol. In a test row, the newestShimadzu white wine „ScienceSelection – Pinot gris late harvestdry“(figure 1), a pinot gris wine,was compared with a dry redwine.

Sample preparation was done byliquid extraction with organic solvent in a milliliter scale. Itneeds only 5 mL sample volumeand 2 mL solvent to give reliableresults. In a first step, the alcoholswere identified in the chromato -gram. A calibration mixture of astandard solution and an internalstandard solution, created in awine matrix with pH = 3.5, wasused. 2-Butanol was applied as aninternal standard (ISTD) and the

method to elevate the enjoymentof their wines ...

Literature[1] Oenology research, Winetech Technical,

How higher alcohols and volatile phe-

nols impact on key aromas, Russell

Moss, 2015.

[2] https://glossar.wein-plus.eu/methanol

[3] https://glossar.wein-plus.eu/

essigsaeure-ethylester

Conclusion

With identification of alcoholsand other organic compounds, it is possible to support aromaprofiling of wines and to monitortheir quality. GC-2030 with FIDdetection offers an efficient wayto reliably analyze these withoutthe need for advanced equipmentand complicated sample prepara-tion. For winemakers, a helpful

concentrations of the compoundsin the calibration mixture were inthe range of 50 to 200 mg/L.

Table 1 shows the parameters ofthe GC method. Analysis timewas optimized at 25 min. As col-umn, a SH-Rxi-624Sil MS of 30 mlength, 0.25 mm ID and 1.4 µm dfwas used.

In the second step, the cold winesample, added with internal stan-dard solution, was vortexed withNaCl and dichloromethane; phase

separation was doneat room temperaturefollowed by centri -fugation. The driedor ganic phase isready for injection.

Quantification oftarget compoundswas done via re -sponse factors, cal-culated from theareas and concentra-tions of the calibra-tion mixture. Withthese response fac-tors, concentrationsof alcohols in thesample were calcu-lated.

Results

Table 2 summarizesthe results for bothwines measured, andfigure 2 shows achromatogram ofthe Shimadzu wineanalyzed.

Both wines tested showed similarvalues for n-pro panol and ethylacetate. The main differences werefound for metha nol, isobutanoland isoamyl alcohol, showingmuch higher amounts in the redwine. These results correlate toaverage concentrations of metha -nol in red and white wines as stat-ed in the literature. According to[3], about 60 to 230 mg/L metha -nol in red wines and 17 to 100 mg/Lin white wines are present.Furthermore, a common methodfrom the OIV (InternationalOrganization of Vine and Wine)for methanol analysis providedsimilar results in their validationtests of the methanol analyticmethod for GC.

Pinot grislate harvest dry

14 % vol. / 0.375 LSpecial German quality wine 2017

Bottled by the proprietor A.P.NR 941/03/18Winery by Herbert Engist, Winzerweg 6

79235 V.-Achkarren, Germany, contains sulphites

Science Selection

Figure 1: Shimadzu wine »Science Selection – Pinot gris

late harvest dry«

Table 2: Concentration in mg/L of alcohols and ethyl acetate in both wines analyzed

Table 1: Method parameters for alcohols and ethyl acetate in wine

Figure 2: Chromatogram of the Shimadzu wine analyzed

0

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30,000

40,000

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80,000

90,000

uV

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Uwe Karst holds the Chair of AnalyticalChemistry at the University of Münster inGermany. After diploma and Ph.D. studies in Münster, which he finished in 1993, hejoined the University of Colorado in Boulderas postdoctoral associate. He returned toMünster to obtain his habilitation and wasappointed as Full Professor of ChemicalAnalysis at the University of Twente in theNetherlands from 2001 to 2005, after whichhe assumed his current position.

He is author of more than 250 publicationsin peer-review journals and 18 patents.Together with his research group, Prof. Karsthas organized several international andnational conferences including the Interna -tional Symposium on Chromatography in2008, the Metallomics Conference in 2011and the European Winter Conference onPlasma Spectrochemistry in 2015.

LATEST NEWS

We have been collaborating withthe EUIC on imaging for morethan a year, and a major topic atthis moment is further improve-ment of the combination of laserablation and ICP-MS for chemicalimaging purposes. As in otherprevious and current cooperationswith various instrument manufac-turers, we see our role not only in developing applications, butalso in contributing to the furtherdevelopment of the actual andfuture instrument generations.This also includes suggestions forimproved hardware, software forinstrument control, data evalua-tion and integration of the instru-ment´s data with data of otherimaging methods. Within our cur-rent project, the focus is directedon LA-ICP-MS and its combina-tion with MALDI-MS and

S himadzu’s European Inno -vation Center (EUIC)merges cutting-edge analyti-

cal technologies of Shimadzu withgame-changing topics and expert-ise from leading scientists. Thisinnovation-oriented cooperationfocuses on creating new solutionsfor tomorrow.

The European Innovation Centerapplies a decentralized structureall over Europe to be in close localproximity to scientists and relatedmarkets.

With their leading-edge researchexpertise, highly-reputed scientistsfrom well-known European uni-versities cover the academic partof the EUIC. Their scientificfocus areas include clinical appli-cations, imaging technology, foodand composites, with an emphasison new methods, tools, techniques,diagnostics and solutions.

This issue of Shimadzu NEWScovers an interview with ProfessorUwe Karst, University of Müns -ter, Germany. With a focus onimaging technology within theEUIC, he gives insights on hiscurrent research projects.

To start, can you outline the research you conduct ingeneral? What is currentlystate-of-the-art?

Our group specializes in thedevelopment and application ofanalytical methods and instrumen-tation to address complex analyti-cal problems, originating mainlyfrom the biomedical area.

tion-mass spectrometry (MALDI-MS) and related techniques toobtain distribution informationabout intact molecules, while dis-tribution and quantification of theelements is accessible by laserablation (LA) coupled to ICP-MSand micro-X-ray fluorescence(µXRF). As an example, investiga-tion of side effects of Cisplatin-based tumor therapy requires spe-ciation analysis to detect andquantify the individual platinumspecies formed in body fluids andtissues, while imaging by LA-ICP-MS provides quantitative distribu-tion information on platinum inhuman or animal tissues.

Can you describe the research you are doing at theEuropean Innovation Centerwith Shimadzu?

One of our major research areas is speciation analysis. The needfor speciation analysis is causedby the fact that the physiologicalproperties (uptake, distribution,metabolism and excretion) ofmetal-containing compounds arestrongly dependent on the indi-vidual metal species rather than on the heteroatom in general. This is easily proven using theexample of hexavalent chromium,which is considered to be toxicand carcinogenic, while trivalentchromium is regarded as a possi-ble essential trace metal species.

A second major research area ofour group is chemical imaging –analysis of the distribution andspatially resolved quantification of low molecular weight analytesin biological matrices.

How much are speciation analysis and chemical imaginglinked to each other?

Speciation analysis and chemicalimaging complement each otherperfectly regarding the analysis of metal species in the organismsof humans, animals and plants.

Speciation analysis mostly usesliquid phase separations to sepa-rate the metal or metalloid speciesprior to identification by electro-spray mass spectrometry (ESI-MS) and quantification by induc-tively coupled plasma-mass spec-trometry (ICP-MS).

Chemical imaging, on the otherhand, is carried out by matrix-assisted laser desorption/ioniza-

14 SHIMADZU NEWS 3/2018

Multimodal imaging by elemental and molecular massspectrometryEuropean Innovation Center – Interview with Prof. Uwe Karst, University of Münster (Germany)

LATEST NEWS

15SHIMADZU NEWS 3/2018

the manufacturers as well). I justcame back from a large Radiologycongress which Shimadzu alsoattended, presenting equipmentfor medical imaging at theirbooth. While we have been usingchromatography (LC, GC) andspectroscopy (UV/vis, fluores-cence, AAS) instrumentation fromShimadzu for more than 20 yearsfor research and education, ourcooperation in the imaging fieldwas established only three yearsago, and is currently centeredaround LA-ICP-MS and comple-mentary MALDI-MS work.

What are Shimadzu’s strengthscompared to other vendors (notlimited to the instruments)?

Cooperation is always based ontrust and on personal relations,and a major reason for us to workwith Shimadzu equipment at alarger scale during my habilitationphase, in which I had very limitedequipment, was an excellent rela-tion with the local sales agent. He was always helpful to a muchlarger extent than we couldexpect, and he was just an out-standing ambassador for the com-pany.

Of course, well-performing androbust instrumentation helps aswell, but the more complex theanalytical challenges become, themore important is excellent com-munication and cooperationbetween individuals on both sides.Additionally, in our current situa-tion, a broad spectrum of imaginginstrumentation from any manu-facturer is particularly attractiveto us due to the complexity of our analytical problems and theincreased chances to tackle themost difficult challenges.

Could you share any requeststhat you have with respect to analytical and measuringinstrument vendors?

Let me start with a very generalstatement that is not addressed toany particular vendor: While theworld of analytical challenges isconverging more and more, evenincluding a vanishing “wall”between “organic” and “inorgan-ic” analysis, there are often busi-

MALDI-MS/MS, as many of ourcurrent analytical challenges re -quire the combined use of com-plementary imaging techniques.

Why are you interested in this research? What is the goal?Why is it important?

The analysis of low molecularweight compounds with physio-logical effects is currently (andprobably always will be) an areaof high complexity and individualanalytical solutions. In contrast toOmics techniques, the potentialfor automation of procedures forhigh-throughput analysis is limit-ed due to the strongly varyingchemistry behind each analyticalproblem we are facing.

However, this chemical variabilityand the need to address challengeswith a combination of technologyand chemistry is exactly what Ilike in this field of research. Foreach question, there is a plethoraof possible approaches to bechecked, and interdisciplinaryteams with colleagues from Medi -cine and Biology have to cooper-ate well to be successful. Evenduring my postdoctoral times, I would never have expected to be able to contribute to investiga-tions on the side effects of plati -num cancer chemotherapy, on thedeposition of gadolinium frommagnetic resonance imaging (MRI)contrast agents in the human brainor on fibrosis caused by certaintypes of nanoparticles in the lung.

Even more exciting, the combina-tion of chemical and medicalimaging opens up completely newroutes for research. MRI, comput-ed tomography (CT) or positronemission tomography (PET) arehighly complementary regardingin vivo/in vitro situation, spatialresolution, limits of detection andcapabilities for quantification.

How do Shimadzu instrumentssupport your research?

As stated, combined imaging tech-niques are particular intriguing.Cooperation with manufacturersactive in the fields of chemicalimaging are therefore particularlyattractive to us (and hopefully for

ness decisions of instrument ven-dors that lead to fragmentation ofproduct lines and separation ofbusiness units that are hard tounderstand in the light of theincreasing complexity of analyticalchallenges. Sometimes I wish thatscientists were more involved inbusiness decisions of instrumentvendors, as this is not just a mat-ter of rapid sales but also of long-term business relations and busi-ness development in a complexmarket situation. It may be naiveto think that sometimes, wiselong-term decisions should over-rule rapidly profitable decisions,but it would accelerate technicalprogress so much …

Back down to earth again, mywish would be that manufacturersimprove integration of their majorproduct lines to a larger extent,which would be beneficial espe-cially in our research areas of spe-ciation analysis and chemicalimaging. This is one of the majorfactors we are trying to contributeto in our cooperation with theShimadzu European InnovationCenter on imaging.

Take a look into the future:What will happen in the imag-ing field and how will thechange influence the instru-ments/procedures in ten years?

In my opinion, this goes verymuch in line with my reply toyour earlier question: I am awarethat your major markets of todayare not the research areas whichwe are currently working on andthat your sales will go mostly tothe mass markets in routine labs.However, we are facing anincreasing degree of complexity,and being prepared to address thissituation will become even moreimportant in the future. While themedical imaging area will continueto expand due to its immediateand obvious benefit for thepatient/customer, the chemicalimaging area is harder to predict,as the immediate necessity for thepaying customer is not as clear,thus hampering large investmentsin this field.

Regarding scientific content, therewill be massive progress in chemi-

cal imaging, leading to strongoptimism regarding future devel-opment. However, reaching themass markets in routine labs(medical, environmental, food)will require a significant reductionin cost per analysis and for theneed for highly qualified person-nel. This can only be achieved bystrong improvements in speed ofanalysis (more spots per second inimaging mode), improved hard-and software integration and pos-sibly even strategic alliancesbetween vendors of complementa-ry instrumentation or betweendifferent divisions of one vendor.

Let me conclude with the state-ment that there is an increasingamount of light on the horizon,but that the full sunrise has to beearned by hard work and smartdecisions in academia and indus-try. We will do our best to con-tribute!

PRODUCTS

A rgent Energy is the UK’sleading supplier of bio -diesel, taking waste fats,

such as used cooking oils, tallowand sewer grease, and turningthem into high quality biofuel forthe freight and transport indus-tries. Despite the huge inherentvariability in the starting materi-als, the company must reliablyand consistently meet strict quali-ty standards relating to the esterand glyceride content of the bio-fuels it produces. Argent Energy’slaboratory in Stanlow near Liver -pool relies on a trio of gas chro-matographs from Shimadzu toanalyze its biodiesel, the latestaddition being a Nexis GC-2030that was installed to increase test-ing capacity and optimize produc-tion methods.

When travelling on a London bus,the journey may just have beenfueled by Argent Energy biodie -

Steve Lindley, QC LaboratoryManager at Stanlow, explained:“During the refinery process, we need to convert all the glyc-

ensure that the legal maximumallowable amount of total glyc-erides in biodiesel (0.2 %) is notexceeded.

sel, perhaps even refined from thecity’s own infamous fatberg, amonstrous blockage that wasremoved and some of it sent tothe company for processing.

From fatberg to fuel

To get from fatberg to fuel,Argent Energy must undertakeseveral rounds of laboratory test-ing – screening of raw materialsarriving at the refineries, in-process testing and analysis of theend product – all overseen by sci-entists working in Stanlow’s pro-duction, QC and R&D laborato-ries.

While the production lab typicallyuses basic titration methods tomonitor the raw starting materi-als, both the QC and R&D labsdepend heavily on gas chromatog-raphy (GC) for process optimiza-tion and end product testing to

16 SHIMADZU NEWS 3/2018

From fatberg to fuelControlling the quality of biofuels with gas chromatography

Biodiesel refinery of Argent Energy in the UK

Truck with biofuel for passenger and freight transport

PRODUCTS

17SHIMADZU NEWS 3/2018

Expansion to Nexis GC-2030

Shimadzu’s GC application spe-cialists evaluated several potentialsolutions for Argent Energybefore recommending the recentlylaunched Nexis GC-2030 dualcolumn instrument with FIDdetectors. For convenience andease of use, the system includestwo autosamplers – one for eachcolumn – enabling overnightanalysis of non-urgent sampleswith instantly-accessible resultsready and waiting in the morning.Lee Knight observed: “Columninstallation is much easier with

that high. This was overloadingthe columns we had, and detectionwasn’t optimal.”

Steve Lindley added: “Combiningtrace and high concentrationanalyses on the same instrumentpresents a challenge for the QClab. With the glycerides, we’relooking at very, very low levels. If we then put samples with a highconcentration of analyte throughthe same system, it can contami-nate the column and yield weirdresults. There was a real need toseparate the two types of testing,and so we got in touch withShimadzu to see what solutionsthe company could offer.”erides into an end product that is

close to 100 % esters. To ensurethat we have achieved this, we useGC to screen for trace amounts ofany remaining glycerides and todetermine the ester content of thebiofuel. We are looking for reallylow levels of triglycerides, and theShimadzu instruments are greatfor this type of work, not leastbecause they support a tempera-ture program of between 270 and400 °C – a real challenge of glyc-eride screening that not manyGCs can handle.”

Leave no trace

Although until recently the QCand research labs at Stanlow haveshared two Shimadzu GC-2010instruments, they have very dif-ferent analytical needs, which haspresented some operational hur-dles. Whereas the QC lab per-forms trace analysis, the researchlab’s main remit is method devel-opment and process design, involv -ing regular handling of samples ofvastly differing composition tothose of the QC team, and therewas a clear need to separate theworkflows.

Lee Knight, Process DevelopmentChemist in the R&D lab, ex -plained: “The composition of thefeedstocks we receive variestremendously. We never get thesame raw material twice, and sowe have to work on a case-by-case basis and vary our processesaccordingly. Today’s raw materialsvary widely in glyceride contentand composition. We now need tolook for anything between 10 and70 % triglyceride in our mid-process samples – it really can be

Argent Energy is the UK’s leadingprovider of renewable transportfuel, supplying biodiesel to thecommercial freight and passengertransport industries.

The company produces biodiesel at sites in Motherwell near Glas -gow, Scotland and Stanlow nearLiverpool, England by refiningwaste oil streams from plants, factories and the food and restau-rant industries.

Laboratory work: testing in the production process and analysis of the final product

Shimadzu’s ClickTek connectorsthan with conventional screwthread fittings, and the inclusionof a light inside the oven meansthat you can actually see what youare doing. The system’s touch-screen operation is straightfor-ward, and so users, whether theyare new to GC or already familiarwith Shimadzu software, can learnhow to use the instrument withlittle more than a day’s training.”

Steve Lindley said: “The supportwe receive from Shimadzu is quitehands-on; its technical specialistsdid a lot of behind-the-sceneswork to identify suitable startingconfigurations and set-ups, and

will always speak to us on thephone, via email, or even drop in to the lab. The Nexis isShimadzu’s latest GC system,offering even better detectioncapability and greater sensitivityfor our work. Having a third GCwill relieve the burden on theother instruments and allow us toseparate trace and high concentra-tion analyses.”

An early adopter

The Nexis GC-2030 is still a rela-tively new addition to the ArgentEnergy lab bench, having been

installed just a few months ago,and the company is exploring itscapabilities for existing andpotential applications. SteveLindley commented: “We wereone of the first companies in theUK to take delivery of a NexisGC-2030, and we’re experiment-ing with how we will use thesystem in the long term. At themoment, we’re running two dif-ferent columns to see which onegives us the best results; it maybe that we find one type is bestfor samples with high analyteconcentrations and another forlow concentrations.”

Future plans

Moving forward, the plan is tocontinue to perform trace glyc-eride and ester content analysison the two GC-2010 and use the Nexis to support in-processtesting, method developmentand process development tooptimize the plant operatingconditions. Lee Knight: “We’renow looking at the next steppingstones in method and processdevelopment, which is where themain gains are at present, forexample to understand how theprocessing method can berefined to save on reagent costs,increase throughput and improvequality and consistency, movingtowards a better, more effectivesteady state. It’s a work inprogress, but if we can performfewer treatments of the in-process samples, we would bene-fit from even greater reliabilityof our results. To support allthat, we need to perform moredetailed in-process and feedstockanalysis, which is where theNexis GC-2030 will be a bigadvantage in helping us toachieve our objectives.”

One of the biggest contam-inants is air, and CelticRecycling has invested inan air separation plant, en -abling it to produce recy-cled SF6 in ‘good as new’quality.

Once the cleaned gas hasbeen analyzed and its quali-ty certified by quantitativeGC analysis, it can beresold. Currently, no othercompany in the UK is ableto offer this service.

A bespoke GC system

Celtic Recycling wanted toin crease capacity for PCBanalysis and, at the sametime, introduce GC screen-ing of SF6 which could notbe done using the laborato-ry’s existing instrument.

While PCB testing can be per-formed using a standard GC set-up with an electron capture detec-tor (ECD), SF6 requires a systemtailored to gas analysis. This ledthe company to choose a twin col-umn Nexis GC-2030, takingadvantage of Shimadzu’s state-of-the-art technology and expertisein gas sampling and custom-buildinstrumen tation.

Shimadzu worked with the labo-ratory to customize the system sothat it samples SF6 directly from agas cylinder, using a barrier dis-charge ionization detector (BID)to determine whether any contam-inants are present. Shimadzu’spatented BID is a universal detec-tor that can detect all organic com -pounds except Helium and Neon.

It offers significantly enhancedsensitivity compared to thermalconductivity and flame ionizationdetectors – enabling the detectionof all types of trace components atthe 0.1 ppm level – and incorpo-

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Run time cut, possibilities enhancedNexis GC-2030 quantifies contaminants in oil and gas for recycling

C eltic Recycling, basedin Wales and runningtwo facilities close to

the country’s capital ofCardiff, specializes in therecovery, management andrecycling of redundantheavy electrical equipment.The company is one of asmall number of specialistcontractors that work withNa tion al Grid, which ownsand manages grids for elec-tricity and gas supply inthe UK, and other majorelectricity industry compa-nies to safely remove, dis-mantle and recycle end oflife, oil-and gas-insulatedelectrical equipment.

Both the oil and the gasrecovered from high volt-age electrical equipmentcan be recycled after test-ing to ensure that the levels of anycontaminants are within the speci-fied limits. Celtic Recycling’s lab-oratory in Newport, Gwent, haslong used gas chromatography(GC) to analyze polychlorinatedbiphenyls (PCBs) in insulatingoils but lacked the capability toscreen sulfur hexafluoride (SF6)from gas-filled equipment. Withlegislative changes set to make itmore difficult to import virginSF6, and to increase the demandfor recycled SF6 in the UK, thecompany invested in a dual col-umn Nexis GC-2030 gas chroma -tograph to broaden its GC capa-bilities to include gas analysis andto enhance PCB testing capabili-ties.

Why test for PCBs?

In the past, PCBs were used asdielectric insulating fluids intransformers and other high volt-age electrical equipment. At thetime they were thought of as the‘wonder substance’ because they

have superb insulating propertiesand don’t break down. Their usewas banned in the 1980s after itbecame clear that they were haz-ardous to humans and the environ -ment, however, insulating oil con-taining PCBs is still occasionallyfound as electrical equipment hasa long life span.

While samples that are high inPCBs are very rare, trace level con -tamination may still occur. Typi -cally, this is attributed to PCB-fluids being pumped out and re -placed with an alternative oil tocomply with legislation; any resid-ual PCBs not cleaned out of theequipment, however, cause tracecontamination of the fresh insulat-ing oil. For this reason, all sam-ples received by Celtic Recyclingundergo quantitative GC analysisfor PCBs over the range of 5 to100 ppm, with higher concentra-tions also quantifiable. Samplesbelow the legal limit of 50 ppmcan be reused and recycled, while

any oils containing PCBs abovethis level are treated as hazardouswaste and are destroyed.

The SF6 challenge

Changes made to EU legislationsince 2015 will make it increasing-ly difficult to produce or importnew supplies of SF6, an inert gaswith a global warming potentialmany thousands of times greaterthan carbon dioxide, making itextremely harmful to the environ-ment. SF6-filled equipment can beemptied and the gas recovered andstored, but great care must betaken in case arcing has occurredwithin the equipment, resulting inthe formation of highly toxic con-taminants.

Portable analyzers give a broadindication of any contaminantsthat are present, such as hydrogenfluoride, sulfur dioxide and mois-ture, most of which can be re -moved using molecular sieves.

Figure 1: Shimadzu custom gas chromatograph Nexis GC-2030

19SHIMADZU NEWS 3/2018

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rates unique electrode-preservingplasma generation technology thatensures long-term stability. Toavoid saturating the detector, thedesign incorporates a ‘dump valve’,allowing SF6 to be diverted oncethe substances of interest haveeluted. PCB samples are intro-duced via a split/splitless injector,and analyzed using an ECD.

Reaping the benefits

The Nexis GC-2030 was installedat the end of 2017, and the labora-tory is already seeing the benefits.Not only has it extended the labo-ratory’s GC capabilities to includeSF6 analysis, it also provides addi-tional flexibility as the SF6 andPCB set-ups are installed alongsideeach other in a single instrument.This avoids the need to switch outcolumns and change detectors, orto install two separate instruments,one for each type of analysis. Theinclusion of a BID helps to future-proof the system, as this detector issuitable for many other applica-tions should business needs changein the future.

Previously, GC analysis was per-formed using nitrogen carrier gas,but the laboratory opted to use

helium with the new set-up. Thishas reduced the PCB run timefrom 45 to 22 minutes, significant-ly improving turnaround timesand allowing more samples to berun in the same time period asbefore. The system’s powerfulLabSolutions software enhancesintegration, making it easier todetect small peaks and discernthem from background noise, andresulting in increased PCB sensi-tivity compared to the laboratory’solder instrument.

The laboratory has now estab-lished a quantitative assay to deter -mine the level of any contaminants

in the SF6 gas, improving accuracyfor most compounds from around1,000 ppm using the portable ana-lyzers to single figure ppm withthe Nexis GC-2030. To date, theimplementation of the new GCassay has allowed Celtic Recyclingto recover and certify over 3,000kg of SF6 gas for sale and reuse innew equipment.

Celtic Recycling’s laboratorychemist, Jennifer Rapp, comment-ed: “I am really pleased with thenew system and enjoy workingwith it. It is easy to use, and I cangenerate customized reports thatlook very professional with just a

Figure 2: System set-up

few clicks. Maintenance is quitestraightforward and it is very easyto change columns; having a lightinside the oven is a definite advan-tage – I hadn’t realized how darkthe oven is until now! The productspecialists at Shimadzu have beengreat, providing training and help-ing me to set up the methods. It’s good to know that I can relyon their support.”

Acidic? Basic? Chelating? No problem for inert columns!For reactive substances, inert LC columns are essential for a symmetrical peak shape

I n any chromatographic separa-tion, symmetrical peaks withan ideal Gaussian shape are

preferable. Under standard condi-tions, this can usually be accom-plished in case of neutral substanc -es. However, the examination ofstrongly acidic, basic or chelatingcompounds often leads to so-called “peak tailing“ and thus to a clearly asymmetric peak shape.

In these cases, the right choice ofcolumn is crucial: it should be asinert as possible for ionizable ana-lytes in order to avoid undesiredsecondary interactions with thestationary phase.

The inertness of a column

What exactly is meant by “inert-ness“ of a column? Generally

speaking, inertness means that asfew undesirable interactions aspossible take place between thecolumn and the analyte.

When the three substance proper-ties, acidic, basic and chelatinghave an asymmetric peak form(i.e. with undesirable interactions),it suggests that acidic substancesshow an insufficiently chemically

bound phase or impurities that arecontained in the phase and reactwith acidic substances. An insuffi-ciently chemically bound phasecon tains free silanol groups.Unpro -tonated acids can compete withprotons of protonated silanolgroups. This generates asymmetri-cal peaks. �

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Contaminants in the stationaryphase that can trigger hydrogenbonds, or are basic, can interactwith acidic analytes and lead toasymmetric peaks.

Positively charged basic analytesmay interact with remainingslightly acidic silanol groups onthe stationary phase if they have a negative charge. “Endcapping“,i.e. the blocking of accessiblesilanol groups by trimethylsilylligands, is carried out to reducethis interaction as much as possi-ble.

Column:

Shim-pack GISS C18; (100 mm x2.1 mm I.D., 1.9 µm);Shim-pack GIST C18; (100 mm x2.1 mm I.D., 2 µm)C18 (Competitor column 1); 100 mm x 2.1 mm I.D., 2,7 µm)C18 (Competitor column 2); 100 mm x 2.1 mm I.D., 2.6 µm)Shim-pack GIS RP-Shield; (150 mm x 4.6 mm I.D., 5 µm)Shim-pack GIST C18-AQ; (100 mm x 2.1 mm I.D., 1.9 µm)Shim-pack GIST Phenyl; (100 mm x 2.1 mm I.D., 3 µm)

Asymmetric peaks of chelatinganalytes indicate that metal is pres -ent on the phase which chelatinggroups can approach and poten-tially irreversibly bind. With theundesirable interactions de scribed,strong tailing of the peak occurswhich in the worst case can alsolead to a decrease of the peak area.

Most importantly, a column withlittle inertness is not the same as abad column! Whether or not inert-ness is desired is always specific tothe application. For some analytes,particular polar interactions or

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Figure 1: Chelating test (1 caffeine, 2 hinokitiol) and basic test (1 pyridine, 2 dextro-

metorphan, 3 propyl paraben), measured on the Shim-Pack GISS C18

Figure 3: Chelating test (1 caffeine, 2 hinokitiol) and basic test (1 pyridine, 2 dextro-

metorphan, 3 propyl paraben), measured on the C18 competitor column 1

Figure 2: Chelating test (1 caffeine, 2 hinokitiol) and basic test (1 pyridine, 2 dextro-

metorphan, 3 propyl paraben), measured on the Shim-Pack GIST C18

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met al interactions are advanta-geous to achieve stronger reten-tion.

This article deals exclusively withanalytes for which inert columnsare important. Different columntypes were investigated withregard to their inertness and theirinteractions.

Measurement parameters and methods

Instrument:LC-2040C 3D (Shimadzu)

Figure 4: Chelating test (1 caffeine, 2 hinokitiol) and basic test (1 pyridine, 2 dextro-

metorphan, 3 propyl paraben), measured on the C18 competitor column 2.

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21SHIMADZU NEWS 3/2018

Shim-pack GIST Phenyl-Hexyl;(100 mm x 2.1 mm I.D., 3 µm)

Mobile Phase:

Acid Test: 75 % 0.1 % H3PO4; 25 % ACNChelation test: 60 % 0.1 %H3PO4, 40 % ACNBasic test: 65 % 20 mmolKH2PO4, pH 6,9, 35 % ACNFurnace temperature: 40 °C

Flow rate and injection volumewere adapted to the column dimen -sions.

Results

Differences in the measurementresults of the column tests withregard to inertness were observed.The highest inertness was shownby the Shim-pack GISS C18 andthe Shim-pack GIST C18. Inert -ness is one of their greatest advan-tages. The chromatograms in fig-ures 1 and 2 demonstrate that allpeaks are symmetrical and have ahigh intensity.

This illustrates an extraordinaryinertness in the analysis of reac-tive substances, e.g. stronglyacidic, basic or chelating analytes.Figures 3 and 4 illustrate compar-ative measurements on two differ-ent competitor C18 columns.Compared with figures 1 and 2,the chelating agent hinokitiol andthe basic substance dextrometor-

phan show clear peak tailing and a lower intensity.

The GIS RP-Shield column has apolar functional group embeddedbetween the silica surface and theC18 groups. This allows stabilityeven under 100 % aqueous condi-tions.

In the column test, this propertyis clearly visible in the chromato -

gram in the basic test, since thepeaks, especially the dextrometor-phan peak, are misshapen andasymmetrical (figure 5). On theother hand, for acidic analyteswhich can be measured ideallywith this column, symmetricalpeak forms are obtained.

Compared with the phenyl-hexylcolumn, the phenyl column has noendcapping and therefore offersmore polar interactions. This canbe seen in the chromatograms infigures 6 and 7 when comparingthe analyses of the basic sub-stances on both columns.

Dextrometorphan shows strongtailing on the phenyl columncompared to the phenyl-hexylcolumn; the elution order is even

reversed. This reversal is causedpartly by the different functionalgroups of the phenyl and phenyl-hexyl columns.

Compared to conventional C18columns, the GIST C18 AQ col-umn shows very good retention tohydrophilic polar analytes. It canalso be used with a 100 % aque-ous mobile phase without loss ofretention. The C18 AQ column isvery inert. It shows tailing ofbasic substances due to the freesilanol group present on morepolar phases such as C18 AQ (figure 8).

Conclusion

For the analysis of strongly acidic,chelating or basic substances, aninert column must be used. In theShimadzu range, GIST C18 andGISS C18 show particularly inertproperties. Substances can bemeasured accurately with thesetwo inert columns and show sym-metrical peaks with a high intensi-ty.

If polar interactions are desired inorder to obtain an alternativeselectivity for analytes, the choiceshould fall on one of the differentcolumns with polar interactions inthe Shim-pack range.

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Figure 5: Acidic test (1 Salicylic acid, 2 Methyl parabene, 3 Cinnamic acid) and basic test

(1 pyridine, 2 dextro-metorphan, 3 propyl paraben), measured on the Shim-Pack GIS RP-Shield

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Figure 6: Basic test (1 pyridine, 2 dextrometorphan, 3 propylparaben), measured on the

Shim-pack GIST Phenyl

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Figure 7: Basic test (1 pyridine, 2 dextrometorphan, 3 propyl paraben), measured on the

Shim-pack GIST phenyl-hexyl

Figure 8: Basic test (1 pyridine, 2 dextrometorphan, 3 propyl paraben), measured on the

Shim-pack GIST C18-AQ

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LATEST NEWS

22 SHIMADZU NEWS 3/2018

50th anniversary celebration and future perspectives

Let’s have a party!

O ver 300 guests from all overEurope celebrated the 50th

anniversary of ShimadzuEuropa on September 11, 2018.The fully booked Mer cator Hall in Duisburg, Germany hosted the‘Magic Moments Night’, an eventfeaturing music, show acts, dinner,

speeches, greeting notes and a‘Walk of History.’ The Superviso -ry Board and Executive Boardcame from Japan to party togetherwith the European Shimadzu fam-ily, management of the Shimadzusubsidiaries and distributors fromall over Europe. The program was

hosted by Asli Sevindim, a TVjournalist born in Duisburg, thehometown of the Shimadzu Euro -pa headquarters.

The musical part of the eveningwas covered by members of theDuisburg Philharmonic Orches -

LATEST NEWS

23SHIMADZU NEWS 3/2018

tra. The show act performed by‘Physikanten & Co’ combinedentertainment and science. Usingphysical phenomena, the groupmade the 300 guests laugh, smileand wonder. Giant vortex ringsflew 20 - 30 m, and showed in a rapid sequence of experiments

the fascinating aspectsof carbon dioxide, other

than its threat of being a green-house gas.

Scientific edutainment ideallycombines the worlds of physicsand chemistry, both a part of

Shimadzu’s technological home-base.

For the ‘Walk of History’,Shimadzu collected historic adver-tisements, brochures and photo-graphs from exhibitions covering50 years of corporate history �

LATEST NEWS

24

EBFBarcelona, SpainNovember 21 - 23, 2018bcn.europeanbioanalysisforum.eu

MS-Tage 2018Munich, GermanyDecember 4 - 5, 2018www.shimadzu.de/ms-tage

Klinische DagDeventer, NetherlandsDecember 12, 2018https://www.dz.nl/Paginas/Default.aspx

Material and Objects in direct contact withfoodMilan, ItalyDecember 13, 2018www.packagingmeeting.it

Ministerial Conference on Nuclear Science andTechnologyVienna, AustriaNovember 28, 2018www.iaea.org/events

EMEC19Royat, FranceDecember 3 - 6, 2018https://emec19.sciencesconf.org/

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ration, emphasized in his wel-coming speech the importance of the European market whereShimadzu is represented in allcountries and employs about 750 people. The President andCEO of Shimadzu Corporation,Teruhisa Ueda, sent his bestwishes to the workforce anddescribed Shimadzu Europa as

in Europe. These items bridgedthe gap between then and now. A corporate chronicle of 100pages put the development ofShimadzu Europa in the contextof technological, economic, polit-ical and social change in Europe.

Akiro Nakamoto, Chairman ofthe Board of Shimadzu Corpo -

a strong and creative voice in theglobal organization, employingover 11,000 people worldwide.Jürgen Kwass, Managing Direc -tor of Shimadzu Europa, men-tioned that an anniversary is a time to party, as well as an op -portunity to review and recapwhat has been accomplished inthe past, in order to draw the

right conclusions for future goalsand developments. He stated:Shimadzu has the best skilledpeople, innovative products andan excellent distribution networksupporting the future plan tosoon offer 1,000 jobs in Europe.