Latest Update for Food and Environmental from Waters · 2019. 12. 16. · Refreshed Xevo TQ-S micro...
Transcript of Latest Update for Food and Environmental from Waters · 2019. 12. 16. · Refreshed Xevo TQ-S micro...
©2019 Waters Corporation 1COMPANY CONFIDENTIAL
Latest Update for Food and Environmental from Waters
2019 Food and Water Summit, 11-12th September 2019
Dr. Peter Hancock
©2019 Waters Corporation 2COMPANY CONFIDENTIAL
Leading Scientific OrganizationTechnology Provider
Understand market needs
Monitor & assess market trends
Meet regulatory requirements
Address analytical challenges
Introduce innovative technology
Waters’ Role in Food and Environmental Testing
Shared responsibility
Capacity building
Educational programs
Network creation
Partnerships
©2019 Waters Corporation 3COMPANY CONFIDENTIAL
Regulatory
Requirements
Future Directions
and Trends
Emerging Risks
and scares
Current Analytical
Challenges
• Sample diversity and complexity
• Sensitivity, selectivity and speed of analysis
• Direct or point of use analysis
• Contaminant scares
• Consumer/Trade Protection
• Toxicological assessments
• Researching links between food, nutrition and health
• Technological developments for analyte detection
• Improving data management/use of digital information
Understanding Needs
• Permitted limits; banned contaminants
• Validation and Analytical QC
• Reference methods
©2019 Waters Corporation 4COMPANY CONFIDENTIAL
Regulatory
Requirements
Future Directions
and Trends
Emerging Risks
and scares
Current Analytical
Challenges
• Sample diversity and complexity
• Sensitivity, selectivity and speed of analysis
• Direct or point of use analysis
• Contaminant scares
• Consumer/Trade Protection
• Toxicological assessments
• Researching links between food, nutrition and health
• Technological developments for analyte detection
• Improving data management/use of digital information
Understanding Needs
• Permitted limits; banned contaminants
• Validation and Analytical QC
• Reference methods
©2019 Waters Corporation 5COMPANY CONFIDENTIAL
TQ-S cronos
New
Accessible reliable performance
TQ-S micro
Refreshed
Sensitive, flexible and compact
What is the new TQ family for 2019?
Ultimate sensitivity and flexibility
TQ-XS
©2019 Waters Corporation 6COMPANY CONFIDENTIAL
Xevo TQD, Xevo TQ-S cronos, Xevo TQ-S micro
Sensitivity comparison for some pos ion pesticides
5x
15x
4x
15x
3x
12x
Xevo TQ-S micro peak area
Xevo TQ-S cronos peak area
Xevo TQD peak area
1x
1x
1x
Aztrazine-desethyl
Dicrotophos
Methamidophos
©2019 Waters Corporation 7COMPANY CONFIDENTIAL
Xevo TQD, Xevo TQ-S cronos, Xevo TQ-S micro
Sensitivity comparison for some neg ion pesticides
11x
55x
13x
47x
8x
34x
Xevo TQ-S micro peak area
Xevo TQ-S cronos peak area
Xevo TQD peak area
1x
1x
1x
Fluazinam
Fludioxynil
Lufenuron
©2019 Waters Corporation 8COMPANY CONFIDENTIAL
Why is glyphosate (and other polar pesticides) such a
challenge to analyse?
Method Step Challenges
Sample Preparation
Glyphosate is very polar, water soluble and insoluble in organic
solvents, and will bind to metal ions, therefore making the extraction
possibilities limited. Derivatization can be very time consuming
SeparationInsufficient retention on column using reverse phase, requires
derivatization, HILIC or IEX stationary phase
Analysis
Within the extract, other water soluble matrix compounds can also be
found (proteins, sugars, amino acids, salts, etc.) that interfere with the
determination of glyphosate. The use of derivatization is not compound
specific and can lead to selectivity issues
Glyphosate used as a desiccant on cereal crops to aid harvest-results in increased
frequency of residues in products such as bread and breakfast
cereals and beer
©2019 Waters Corporation 9COMPANY CONFIDENTIAL
AMPAGlufosinateGlyphosate
Extended scope of analytes related to glyphosate
Parents:
Glyphosate
Glufosinate
Ethephon
Fosetyl aluminum
Metabolites:
N-acetylglyphosate, aminomethylphosphonic acid (AMPA), n-acetylAMPA
N-acetylglufosinate, 3-methylphosphinicopropionic acid (MPP)
Regulated residue definitions:
mg/kg in
wheatGlyphosate Glufosinate* Fosetyl al**
EU 10 0.03 2
US 30 - -
China 5 - -
* Glufosinate residue definition must report the sum of glufosinate, its salts
MPP and NAG, expressed as glufosinate equivalents.
** Fosetyl aluminum must report the sum of fosetyl, phosphonic acid and their
salts, expressed as fosetyl.
Anionic polar pesticide compounds
©2019 Waters Corporation 10COMPANY CONFIDENTIAL
Our journey to the NEW Anionic Polar Pesticide Column
➢ Mixed mode
Retention
Separation of critical pairs
➢ HILIC type: DEA
Retention
Excellent separation of critical pairs
Retention time stable
Perchlorate compatible
➢ HILIC type (polyvinyl alcohol)
Retention
Acceptable separation of critical pairs
Retention time unstable
Perchlorate incompatible (5 min wide peak)
Retention
RSDs > 20% in different commodities
Lemon Wheat flour
AMPA
Fos Al
Retention time stability
Glyphosate
13.94 min 12.70 min
Separation
©2019 Waters Corporation 11COMPANY CONFIDENTIAL
Waters Anionic Polar Pesticide Column
– 5 µm BEH DEA Particle Technology
– 2.1 x 100mm UPLC Hardware
Enhancements have enabled:
– Extended Peak Shape Integrity
– Maintain Key Analyte Separations
– Retention Without Derivatization
– Reliable Low-Level Detection
– No Sodium EDTA wash
– No need for high levels of buffers
What it is the APP column and why?
5 µm
1.7 µm
8.5 X
5 µm
1.7 µm4.5 X
AMPA
Glyphosate
©2019 Waters Corporation 12COMPANY CONFIDENTIAL
Retention: Analyte retention, without derivatisationRetaining analytes to maximise performance
Time1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00 9.50 10.00 10.50 11.00 11.50 12.00 12.50
%
0
100
t0 = 0.48min
Minimum acceptable RT for the analyte(s) should be at minimum twice the RT
corresponding to the void volume of the column (SANTE/11813/2017)
©2019 Waters Corporation 13COMPANY CONFIDENTIAL
Separation: Critical separations to avoid false detectionsIsobaric interferences from targeted analytes
AMPA
fosetyl-al
phosphonic acid
Separation of fosetyl isobaric
interference in AMPA and
phosphonic acid MRM transitions.
110 < 63
109 < 63
81 < 63
©2019 Waters Corporation 14COMPANY CONFIDENTIAL
min5.050 5.100 5.150 5.200 5.250 5.300 5.350 5.400 5.450 5.500 5.550 5.600 5.650 5.700 5.750
%
0
100
HPEU_021_220819_120
QuPPe Flour 2.5 ng/mLGlyphosate
5.35
1378
min
%
0
100
HPEU_021_220819_120
QuPPe Flour 2.5 ng/mLGlyphosate
5.35
1580
Spike equivalent to 0.010 mg/kg
min2.850 2.900 2.950 3.000 3.050 3.100 3.150 3.200 3.250 3.300 3.350
%
0
100
HPEU_021_220819_120
QuPPe Flour 2.5 ng/mLGlufosinate
3.05
233
2.85
min
%
0
100
HPEU_021_220819_120
QuPPe Flour 2.5 ng/mLGlufosinate
3.05
307
Detection: Detecting, Identifying and QuantifyingAccurately, well below current MRLs
0.010 mg/kg – 0.400 mg/kg wheat flour matrix matched
Glu
fos
ina
teG
lyp
ho
sa
te
Compound name: Glyphosate
Correlation coefficient: r = 0.999119, r^2 = 0.998238
Calibration curve: 530.208 * x + 72.8129
Response type: External Std, Area
Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None
Standard Addition Concentration : 0.137329
Conc-0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Res
pons
e
-0
20000
40000
Conc
Res
idua
l
-5.0
0.0
5.0
10.0
Compound name: Glufosinate
Correlation coefficient: r = 0.999725, r^2 = 0.999451
Calibration curve: 129.083 * x + -39.8463
Response type: External Std, Area
Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None
Conc-0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Res
pons
e
-0
2500
5000
7500
10000
12500
Conc
Res
idua
l
-5.0
-2.5
0.0
2.5
5.0
©2019 Waters Corporation 15COMPANY CONFIDENTIAL
Refreshed Xevo TQ-S micro provides
– Update to the detector to improve performance for small
negative ionizing daughter ions (<m/z 150)
– Enhancements to MassLynx quan workflow
Time3.40 3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00
%
0
100 Glyphosate m/z: 168 > 63
3.5 fold increase in peak area
Xevo TQ-S micro
Refreshed Xevo TQ-S micro
Detection: Achieving default MRL on Xevo TQ-S microEnhanced Xevo TQ-S micro and column showing small can be powerful
Gly1: Gly
©2019 Waters Corporation 16COMPANY CONFIDENTIAL
Reference retention time (TRef) TRef± 0.1
Tomato | Cucumber | Wheat flour
Reliability: Retention time stabilityRetention times you can rely on
Reliable retention times, even between matrices, without significant column conditioning or maintenance.
©2019 Waters Corporation 17COMPANY CONFIDENTIAL
Regulatory
Requirements
Future Directions
and Trends
Emerging Risks
and scares
Current Analytical
Challenges
• Sample diversity and complexity
• Sensitivity, selectivity and speed of analysis
• Direct or point of use analysis
• Contaminant scares
• Consumer/Trade Protection
• Toxicological assessments
• Researching links between food, nutrition and health
• Technological developments for analyte detection
• Improving data management/use of digital information
Understanding Needs
• Permitted limits; banned contaminants
• Validation and Analytical QC
• Reference methods
©2019 Waters Corporation 18COMPANY CONFIDENTIAL
Mass Spectrometric Profiling
Direct MS
• Minimal sample preparation
• No chromatography, Ambient ionisation
• Spatially well defined
• Few hundred species in 1-5 sec
Traditional
• Sample preparation
• GC-MS, GC-MS/MS
• LC-MS, LC-MS/MS
• Few thousand species in 5-30 min
©2019 Waters Corporation 19COMPANY CONFIDENTIAL
Direct analysis of;
– Solids & powders (black tea, spices, etc)
– Liquids (edible oils, whiskey, milk, etc)
– Tablets
– Vapour / aroma
Automation using 12 position
Quick strip cards, Dip-it and SPE-it sampling
DART QDa sample introduction techniques
©2019 Waters Corporation 20COMPANY CONFIDENTIAL
Sample preparation
0.2 g honey
Add 1 mL of ultrapure water
Warm (45oC), vortex mix 30 s
Add 9 mL of 50:50 MeCN: MeOH
Vortex mix 30 s
Roller shake ~ 5mins
Centrifuge @ 6000 rpm for 5 mins
Remove 1 mL supernatant
Dispense 3 µL onto Quickstrip and
allow to dry
Honey samples
1. Light brown / set
2. Yellow / set
3. Yellow / set
4. Dark brown / runny
5. Honey supplement
(light brown / runny)
DART/QDa, Honey authenticity example
©2019 Waters Corporation 21COMPANY CONFIDENTIAL
Honey sample 4 and solvent blank overlay
Showing unique feature regions
Monosaccharides[M+H]+ , [M+nH2O]+
Disaccharides[M+H]+ , dehydration products
Oligosaccharides[M+H]+ ,dehydration productsFlavonoids
Helium
DART+
Desorption temp: 350oC
Rail speed: 0.8 mm/min
Cone voltage: 10 V
Mass range: m/z 100 – 600
Acquisition: Continuum
Sampling frequency: 2 Hz
Gain: 1
©2019 Waters Corporation 22COMPANY CONFIDENTIAL
Honey profile
DART QDa positive ionisation mode He gas @ 350oC
Adulterated honey sample
Authentic honey sample 1
Authentic honey sample 2
Authentic honey sample 3
Authentic honey sample 4
©2019 Waters Corporation 23COMPANY CONFIDENTIAL
LiveID 1D Loadings plot, PCA/LDA 3D Scores Plots
PCA/LDA model
PCA model
©2019 Waters Corporation 24COMPANY CONFIDENTIAL
Extracted ion chromatograms for ion at 390.1
Sample 1 (authentic honey)
Sample 5 (adulterated honey)
Full scan spectral overlay
380 – 397 m/z
Solvent blank – red
Authentic honey – green
Adulterated honey - purple
©2019 Waters Corporation 25COMPANY CONFIDENTIAL
Regulatory
Requirements
Future Directions
and Trends
Emerging Risks
and scares
Current Analytical
Challenges
• Sample diversity and complexity
• Sensitivity, selectivity and speed of analysis
• Direct or point of use analysis
• Contaminant scares
• Consumer/Trade Protection
• Toxicological assessments
• Researching links between food, nutrition and health
• Technological developments for analyte detection
• Improving data management/use of digital information
Understanding Needs
• Permitted limits; banned contaminants
• Validation and Analytical QC
• Reference methods
©2019 Waters Corporation 26COMPANY CONFIDENTIAL
Perfluoroalkylated Substances (PFAS)
PFAS = PFC = AFFF
First created in the 1930s
Widespread applications
– Non stick coatings, surfactants, packaging, firefighting foams
– Polymerization aid for polytetrafluoroethylene (PTFE) and
other fluoropolymers
Stable and persistent in the environment (POP)
– Bio-accumulative
Identified in environmental samples worldwide
– Found in arctic polar bears
– Most humans have a range of PFAS in their blood
PFOS and PFOA most studied PFAS compounds but 1000’s have
been created
Perfluoro Carboxylic Acid
(PFOA)
Perfluoro Sulfonic Acid
(PFOS)
©2019 Waters Corporation 27COMPANY CONFIDENTIAL
Worldwide Interest in PFAS
©2019 Waters Corporation 28COMPANY CONFIDENTIAL
EPA Method
537*
ISO
25101
ASTM
7979
Sample Prep SPE SPE Dilute, Filter
Injection Volume 1 - 10 µL 1 - 10 µL 30 µL
Instrument sensitivity
requiredXevo TQ-S micro Xevo TQ-S micro Xevo TQ-XS
Number of
compounds18 2 24
Comparison of analysis methods
*EPA 537 is for drinking water analysis only
©2019 Waters Corporation 29COMPANY CONFIDENTIAL
463>369
463>369
Time2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50
%
0
100
2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50
%
0
100
100 pptPFOA standard
Blank injection
BackgroundPFOA
PFOA
PFAS’s Interferences/Contamination
©2019 Waters Corporation 30COMPANY CONFIDENTIAL
Solvent
Flow
PEEK
Tubing
Stainless
Steel Coil
Isolator
Column
Waters PFC Kit
©2019 Waters Corporation 31COMPANY CONFIDENTIAL
Time2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00
%
0
100
2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00
%
0
100
Nopeaks
Background PFOA contaminant
Background PFOA contaminant
PFOA
Blank Injection
300 pptPFOA standard
0.5min
MRM Chromatograms of PFOA
With PFC Kit Installed
©2019 Waters Corporation 32COMPANY CONFIDENTIAL
ASTM 7979-17
Sample Prep:
5 mL sample + 5 mL
methanol
2 g sample + 10 mL
1:1 water : methanol
Adjust pH to ~ 9-10
Shake 1 hour
Syringe filter entire
sample
Acidify and transfer to
polypropylene vial
WA
TE
R
AS
TM
7979
SO
IL
AS
TM
7968
Sample Pre-
Treatment
WaterSurface
Ground
Influent
Effluent
SoilsSand
Silt
Lean Clay
Fat Clay
©2019 Waters Corporation 33COMPANY CONFIDENTIAL
Compounds Included in Methods
Carboxylates
C4 – C14, C16, C18
Sulfonates
C4 – C10
Others
4:2/6:2/8:2 FTS FHEA/FOEA/FDEA
FHUEA FHpPA
FOUEA
PFecHS
diPAP
Emerging
GenX ADONA
11Cl-PF3OUdS 9Cl-PF3ONS
PFEESA
PFMBA
NFHDA
FOSA
NMeFOSAA/NEtFOSAA
NMeFOSA/NEtFOSA
©2019 Waters Corporation 34COMPANY CONFIDENTIAL
Source Parameters
Instrument: Xevo TQ-XS
Ion Mode: ESI-
Capillary Voltage: 1.0 kV
Desolvation Temperature: 500°C
Desolvation Flow: 1100 L/hr
Cone Flow: 150 L/hr
LC Method
Instrument: Acquity I Class with PFC Kit
Column: CSH Phenyl Hexyl 2.1mm x 100 mm, 1.7 µm
Mobile Phase A: 95:5 H2O:MeOH + 2 mMammonium acetate
Mobile Phase B: MeOH + 2 mM ammonium acetate
Injection Volume: 30 uL
Gradient:
Instrument Methods
Time
(min)
Flow
(mL/min)
%A %B
0 0.3 100 0
1 0.3 80 20
6 0.3 55 45
13 0.3 20 80
14 0.4 5 95
17 0.4 5 95
18 0.3 100 0
22 0.3 100 0
MS Method
• Developed using QuanOptimize
• MRMs, CV, CE
• Divert flow to waste from 15 – 21 mins
©2019 Waters Corporation 35COMPANY CONFIDENTIAL
Cal Curve pt 8
Time3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00
%
0
100
PFAS_1Feb18_010 68: MRM of 1 Channel ES- TIC (M4_82diPAP)
9.93e6
Overall Method Summary
ERA certified QC sample injected as control throughout
analysis
Reporting Limit Check
Blank sample + targets &
surrogates. Taken through sample
prep
Detectable recovery
35-150%
Reagent Blanks
50:50 water : methanol + 0.1% acetic
acid
Concentration must be < half reporting limit
Method Blank
Blank sample + surrogates.
Taken through sample prep
Concentration must be < half reporting limit
Lab Control
Blank sample + targets &
surrogates. Taken through sample
prep
Target recovery
70-150%
©2019 Waters Corporation 36COMPANY CONFIDENTIAL
Method Detection Limits (MDL)
Well below the necessary reporting limits for the compounds defined in
ASTM 7979
Reporting Range is the required range the method must be able to cover as defined in ASTM 7979 method
©2019 Waters Corporation 37COMPANY CONFIDENTIAL
Compound name: PFOA
Correlation coefficient: r = 0.999618, r^2 = 0.999235
Calibration curve: 1618.33 * x + 695.974
Response type: External Std, Area
Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None
Conc-0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200
Re
sp
on
se
-0
25000
50000
75000
100000
125000
150000
175000
200000
225000
250000
275000
Curve 3
Time10.90 11.00 11.10 11.20
%
0
100
10.90 11.00 11.10 11.20
%
0
100
PFAS_30Jan19_09 Sm (Mn, 2x2) 34: MRM of 2 Channels ES- 498.9 > 98.9 (PFOS)
9.56e3Area
11.01;566
PFAS_30Jan19_09 Sm (Mn, 2x2) 34: MRM of 2 Channels ES- 498.9 > 79.9 (PFOS)
5.71e3Area
11.01
454
498.9 >
98.9
Linearity and Sensitivity
2.5 ng/L injection
R2 = 0.9992
Curve 3
Time9.75 9.80 9.85 9.90 9.95
%
0
100
9.75 9.80 9.85 9.90 9.95
%
0
100
PFAS_30Jan19_09 Sm (Mn, 2x2) 20: MRM of 2 Channels ES- 412.9 > 368.9 (PFOA)
9.64e4Area
9.82;4407
PFAS_30Jan19_09 Sm (Mn, 2x2) 20: MRM of 2 Channels ES- 412.9 > 168.9 (PFOA)
2.42e4Area
9.82;1327
412.9 >
368.9
Curve 3
Time9.75 9.80 9.85 9.90 9.95
%
0
100
9.75 9.80 9.85 9.90 9.95
%
0
100
PFAS_30Jan19_09 Sm (Mn, 2x2) 20: MRM of 2 Channels ES- 412.9 > 368.9 (PFOA)
9.64e4Area
9.82;4407
PFAS_30Jan19_09 Sm (Mn, 2x2) 20: MRM of 2 Channels ES- 412.9 > 168.9 (PFOA)
2.42e4Area
9.82;1327
412.9 >
168.9
PFOA
Compound name: PFOS
Correlation coefficient: r = 0.998997, r^2 = 0.997995
Calibration curve: 196.264 * x + -39.187
Response type: External Std, Area
Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None
Conc-0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200
Re
sp
on
se
-0
5000
10000
15000
20000
25000
30000
35000
R2 = 0.9980
PFOS
Curve 3
Time10.90 11.00 11.10 11.20
%
0
100
10.90 11.00 11.10 11.20
%
0
100
PFAS_30Jan19_09 Sm (Mn, 2x2) 34: MRM of 2 Channels ES- 498.9 > 98.9 (PFOS)
9.56e3Area
11.01;566
PFAS_30Jan19_09 Sm (Mn, 2x2) 34: MRM of 2 Channels ES- 498.9 > 79.9 (PFOS)
5.71e3Area
11.01
454
498.9 >
79.9
2.5 ng/L injection
Cal 2
Time6.80 6.90 7.00 7.10
%
0
100
6.80 6.90 7.00 7.10
%
0
1006.95;417
6.95;602
Cal 2
Time6.80 6.90 7.00 7.10
%
0
100
6.80 6.90 7.00 7.10
%
0
1006.95;417
6.95;602
285 >
185
285 >
119
Compound name: GenX
Correlation coefficient: r = 0.999417, r^2 = 0.998835
Calibration curve: 29.2932 * x + 274.34
Response type: External Std, Area
Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None
ppt-0 20 40 60 80 100 120 140 160 180 200
Re
sp
on
se
-0
1000
2000
3000
4000
5000
6000
10 ng/L injection
R2 = 0.9988
GenX
©2019 Waters Corporation 38COMPANY CONFIDENTIAL
Regulatory
Requirements
Future Directions
and Trends
Emerging Risks
and scares
Current Analytical
Challenges
• Sample diversity and complexity
• Sensitivity, selectivity and speed of analysis
• Direct or point of use analysis
• Contaminant scares
• Consumer/Trade Protection
• Toxicological assessments
• Researching links between food, nutrition and health
• Technological developments for analyte detection
• Improving data management/use of digital information
Understanding Needs
• Permitted limits; banned contaminants
• Validation and Analytical QC
• Reference methods
©2019 Waters Corporation 39COMPANY CONFIDENTIAL
SELECT SERIES Cyclic IMS is a unique ion mobility
mass spectrometer combining next generation cyclic
ion mobility with a new high performance TOF
Key features of Cyclic IMS
– Higher, variable IMS resolution
– IMS selection of ions
– IMSn multi stage IMS selection and fragmentation
Provides unlimited experimental opportunities
enabling leading researchers to solve the most
challenging analytical problems
Select Series Cyclic IMS
©2019 Waters Corporation 40COMPANY CONFIDENTIAL
Universal Ion SourceESI & nESI
NEW Cyclic IMSHigh/ variable resolution Novel IMSn funcionality NEW Offset Tof
Extended flight path
Dual Gain ADCExtended
dynamic range
XS Collision CellEnhanced transmission
Stepwave XSEnhanced transmission
characteristics
NEW Customised MassLynxWith interactive instrument
control software
©2019 Waters Corporation 41COMPANY CONFIDENTIAL
1 pass
(65 /)
2 passes
(100 /)
4 passes
(140 /)
5 passes
(158 /)
3 passes
(124 /)
IMS Performance Summary
Single and Multi Pass IMS
Trisaccharide mix - all 3 components have the same m/z [527.1588] and can’t be separated by mass spectrometry
Raffinose MaltotrioseMelezitose
*SYNAPT G2-Si, Resolution ~40
©2019 Waters Corporation 42COMPANY CONFIDENTIAL
Delivering new levels of ion mobility performance
50 passes R(CCS/CCS) ~ 500
5 passes R(CCS/CCS) ~ 165
Time (ms)
38 39 40 41 42 43 44 45 46 47 48
360 370 380 390 400 410 420 430 440 450 460
Raffinose
Maltotriose
Melezitose
Cyclic IMS provides extraordinary ion mobility resolution
allowing highly detailed structural information to be obtained
©2019 Waters Corporation 43COMPANY CONFIDENTIAL
Product ion mass spectra of mobility separated (Synapt)
danofloxacin protomers (I) and (II).
Observed mass [m/z]
Inte
nsity [
counts]
CH3
N N
N
F
O+
O
OH H
-H2O
-CH3NH2
N N
N+
F
O
O
O
CH3
H
H
H
-CO2
I
II
-HF
0
5000
10000
15000
20000
25000
30000
35000
40000
45000
1 2 3
Re
spo
nse
Replicate
Enrofloxacin Protomer Response Vs Replicate Spiked Porcine Extract
Enrofloxacin
Enrofloxacin_1
0
5000
10000
15000
20000
25000
1 2 3
Re
spo
nse
Replicate
Ciprofloxacin Protomer Response Vs Replicate Spiked Porcine Extract
Ciprofloxacin
Ciprofloxacin_1
https://doi.org/10.1002/rcm.8371
©2019 Waters Corporation 44COMPANY CONFIDENTIAL
Danofloxacin IM protomer separation using Synapt
(N2 and CO2 IM gas) and cIM (N2 IM gas, 5 passes)
Arrival Time [ms]
4.54
5.56 82.89
92.42
95.96
Synapt N2cIM N2
II
I
II
III
I
II
III
Synapt CO2
5.9
3.84
4.20
I
https://doi.org/10.1002/rcm.8371
©2019 Waters Corporation 45COMPANY CONFIDENTIAL
Protein structureOligosaccharidesTechnology
Breakthrough innovation, driven by science
Multiple peer reviewed publications
Antibiotic residues
©2019 Waters Corporation 46COMPANY CONFIDENTIAL
Waters has commitments as a technology provider and leading scientific
organisation for food and water safety, quality testing and research
Our goal is to understand your food and environmental testing needs and
provide technologies, knowledge and methods to address those needs
– Regulatory requirements
– Analytical challenges
– Emerging risks and food scares
– Future directions and trends
Summary