Chromatography: Automated solid-phase extraction (SPE) for the Environmental Testing Laboratory

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Today’s analytical laboratory is faced with tight deadlines to produce results from testing environmental samples. Too often, solid-phase extraction (SPE) presents a bottleneck in the analytical testing process and may cause poor analyte recoveries and highly variable. Despite advances in analytical instrumentation, sample prep often relies on tedious, manual, and expensive techniques such as liquid-liquid extraction. Sample preparation of environmental water samples can be automated, however.. Use of automated sample preparation addresses the many challenges that laboratories face when preparing samples and can help improve sample processing turnaround times. Chromatography presentation goes with this free on-demand webinar. Link to webinar:

Transcript of Chromatography: Automated solid-phase extraction (SPE) for the Environmental Testing Laboratory

  • 1. 1Automated SPE for the Environmental TestingLaboratoryAaron KettleProduct Manager Thermo Fisher Scientific,Automated SPE Systems9/24/2014The world leader in serving science

2. The Challenge for Analysis21.5 mL GC / LC VialHow do we get analytes out of these samples? 3. The Answer is Sample Preparation Extraction Removes analytes from the sample Eliminates compounds that interfere with the analysis (Clean Up) Evaporation Concentrates extracted analytes for analysis Evaporates extracted samples for re-constitution Most time consuming part of analytical procedure (>60%)* Single largest source of errors in the workflow (>30%)**3*Majors, R.E. LC-GC, 1995, 13, 742-749, and **Majors, R.E. LC-GC, 1999, 17, S8 - S13 4. Analysis Techniques!4 5. Analysis Techniques!5 6. Sample Preparation6 7. Sample Preparation7 8. The Important Parameters for Sample Preparation8 Solvent Use Amount of solvent consumed for the extraction Solvents are expensive; reducing use reduces costs Extraction Time Amount of time required for each extraction to occur Reducing extraction time increases lab throughput % Recovery Amount of analyte recovered following the extraction Low % recovery yields poor analytical results % Relative Standard Deviation (RSD) Measure of reproducibility between extractions Extraction results have greater reproducibility with lower %RSDsThese Parameters Evaluate SP Techniques 9. Solid-Phase Extraction (SPE)9 SPE is one of the simplest, most cost-effective and versatile methods ofsample preparation SPE has been widely used in many environmental and food laboratoriesprior to analysis with GC & GC/MS or LC & LC/MS SPE is primarily performed with inexpensive vacuum pumps, manifolds,and choices of many low-cost, prepackaged, disposable cartridges ordisks. 10. Why is SPE Used?ConcentrationIncreases detectorsensitivity and improvesdetection limits10Clean UpRemoves interferencesprior to the analyticaltechnique Matrix RemovalRemoves matrix and elutesthe sample into a solventcompatible with the analyticaltechnique 11. SPE vs. Liquid-Liquid Extraction (LLE)11 Subject to emulsion formation Incomplete phase separations Poor analyte recoveries Uses expensive breakable glassware Uses great volumes of solvent Must evaporate large volumes ofsolvent Faster and decreases solvent use Can be automated More efficient extraction Many SPE phases to accomplishgreater separation No emulsionsSeparatory Funnel used for LLEThermo Scientific Dionex SolEx SPE Cartridges 12. The Process of SPE12 13. Dionex SolEx SPE Sorbent Substrates13Silica-Based Sorbents Polymeric SorbentsSilica substrate with bound functional groupFunctional group imparts retentive propertiesNamed for character of the functional group(e.g. C18)Styrene-divinyl benzene copolymers that canbe modified to create ion exchangers throughanimation or sulfonationHigh-capacity particles (800 m2/g) with narrowsize (22 m) to produce highly efficient lowback-pressure extractionsActivated CarbonHigh surface area (1000 m2/g) ensuresretention of multiple analytes simultaneouslyHigh capacity particles (60 m) ensuresefficient retention in more challengingmatrices (e.g. waste water) 14. Thermo Scientific Dionex AutoTrace 280 SPE Instrument1447 mm Disk System Cartridge (1, 3 or 6 mL) SystemThe Thermo Scientific Dionex AutoTrace 280 SPE instrument provides reliableautomated SPE for analytical chemists determining organic pollutants in large-volumeaqueous samples. Unlike traditional methods such as liquid-liquid extraction usingseparatory funnels, the Dionex AutoTrace 280 SPE instrument saves time, solvent andlabor ensuring high reproducibility and productivity for analytical laboratories. The unit canprocess up to 6 samples in 2-3 hours. 15. Dionex AutoTrace 280 SPE: For Liquid Samples Reduced sample extraction cost Solvent consumption (up to 90% less than LLE) Labor cost (15 min operator intervention) Improved productivity 6 samples loaded onto cartridges in 15 min Improved analytical precision Automated sample loading and elution Positive pressure displacement156 mL Cartridge System 16. Pesticide Recovery Study16Dionex AutoTrace 280 SPE instrument Produces Higher Recoveriesthan Vacuum Manifold 17. Dionex AutoTrace 280 SPE InstrumentKey Applications Summary17Analytes Determinative Step Matrix Application NotePolyaromatic Hydrocarbons(PAHs)GC-MS Surface Water AN 876Dioxins and Furans GC-MS Surface Water AB 805Polychlorinated Biphenyls(PCBs)GC-ECD Surface Water AB 805Endocrine Disruptors GC-MSSurface WaterDrinking WaterAB 801Semivolatile OrganicCompoundsGC & GC-MS Drinking Water AN 819Organochlorine Pesticides GC-ECD Drinking Water AN 1004Sex Hormones HPLC-UV Drinking Water TN 148Tricolsan HPLC-UV Drinking Water AN 1081Explosives HPLC-UV Ground Water AN 358Linear Alkyl Benzene Sulfonate HPLC-UV Waste Water AN 1080Organophosphorous Pesticides GC-NPD Drinking Water Pending PublicationVisit 18. U.S. EPA SPE 500 Methods18EPA Method Analytes Extraction and Analytical Methods Chemistry Used506 Phthalate and Adipate Esters SPE and GC/PID C18507 N and P containing Pesticides SPE and GC C18508.1Chlorinated pesticides, herbicides andorganohalidesSPE and GC-ECD C18521 Nitrosamines SPE and GC/MS/MS Carbon522 Dioxane SPE and GC/MS Carbon525.2 Semivolatile Organic Compounds (SVOC) SPE and GC/MS C18525.3 Semivolatile Organic mpounds (SVOC) SPE and GC/MS C18526 Semivolatile Organic in DW SPE and GC/MS HRPHS527 Flame Retardants SPE and GC/MS HRPHS528 Phenols SPE and GC/MS HRPHS529 Explosives SPE and GC/MS HRPHS532 Phenylurea SPE and HPLC C18535 Acetic Herbicides SPE and LC/MS/MS Graphitized carbon548 Endothal SPE and GC/ECD C18539 Hormones SPE and LC/MS/MS HRPHS553 Benzidines and N containing Pesticides SPE and LC/MS C18554 Carbonyl compounds SPE and LC C18 19. U.S. EPA SPE 600 /1600 Methods19EPA Method Analytes Extraction and Analytical Methods Chemistry Used606,608, 609,611, 612Organochlorine Pesticides and PCBs SPE and GC/ECD C181613 Dioxins and Furans SPE and GC/MS C181614 Brominated Diphenyl Ehters SPE and HRGCMS C181657 Organophosphorous Pesticides GPC/SPE and GC C181668a PCB and congeners SPE and HRGC/HRMS C181694 Pharmaceuticals & Personal Care Products SPE and LC/MS/MS HRPHS