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The world leader in serving science

Aaron Kettle

Product Manager – Thermo Fisher Scientific, Automated SPE Systems

9/24/2014

Automated SPE for the Environmental Testing Laboratory

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The Challenge for Analysis

1.5 mL GC / LC Vial

How do we get analytes out of these samples?

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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%)**

*Majors, R.E. LC-GC, 1995, 13, 742-749, and **Majors, R.E. LC-GC, 1999, 17, S8 - S13

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Analysis Techniques!

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Analysis Techniques!

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Sample Preparation…

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Sample Preparation…

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The Important Parameters for Sample Preparation

• 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 %RSDs

These Parameters Evaluate SP Techniques

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Solid-Phase Extraction (SPE)

• SPE is one of the simplest, most cost-effective and versatile methods of sample preparation

• SPE has been widely used in many environmental and food laboratories prior 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 or disks.

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Why is SPE Used?

Concentration

Increases detector sensitivity and improves detection limits

Clean Up

Removes interferences prior to the analytical techniqueMatrix Removal

Removes matrix and elutes the sample into a solvent compatible with the analytical technique

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SPE vs. Liquid-Liquid Extraction (LLE)

• Subject to emulsion formation

• Incomplete phase separations

• Poor analyte recoveries

• Uses expensive breakable glassware

• Uses great volumes of solvent

• Must evaporate large volumes of solvent

• Faster and decreases solvent use

• Can be automated

• More efficient extraction

• Many SPE phases to accomplish greater separation

• No emulsions

Thermo Scientific™ Dionex™ SolEx ™ SPE Cartridges

Separatory Funnel used for LLE

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The Process of SPE

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Dionex SolEx SPE Sorbent Substrates

Silica-Based Sorbents Polymeric Sorbents

Silica substrate with bound functional group

Functional group imparts retentive properties

Named for character of the functional group (e.g. C18)

Styrene-divinyl benzene copolymers that can be modified to create ion exchangers through animation or sulfonation

High-capacity particles (800 m2/g) with narrow size (22 µm) to produce highly efficient low back-pressure extractions

Activated Carbon

High surface area (1000 m2/g) ensures retention of multiple analytes simultaneously

High capacity particles (60 µm) ensures efficient retention in more challenging matrices (e.g. waste water)

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Thermo Scientific Dionex AutoTrace 280 SPE Instrument

The Thermo Scientific™ Dionex™ AutoTrace 280 SPE instrument provides reliable automated SPE for analytical chemists determining organic pollutants in large-volume aqueous samples. Unlike traditional methods such as liquid-liquid extraction using separatory funnels, the Dionex AutoTrace 280 SPE instrument saves time, solvent and labor ensuring high reproducibility and productivity for analytical laboratories. The unit can process up to 6 samples in 2-3 hours.

47 mm Disk System Cartridge (1, 3 or 6 mL) System

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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 displacement

6 mL Cartridge System

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Pesticide Recovery Study

Dionex AutoTrace 280 SPE instrument Produces Higher Recoveries than Vacuum Manifold

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Dionex AutoTrace 280 SPE Instrument

Analytes Determinative Step Matrix Application Note

Polyaromatic Hydrocarbons (PAHs) GC-MS Surface Water AN 876

Dioxins and Furans GC-MS Surface Water AB 805

Polychlorinated Biphenyls (PCBs) GC-ECD Surface Water AB 805

Endocrine Disruptors GC-MS Surface WaterDrinking Water AB 801

Semivolatile Organic Compounds GC & GC-MS Drinking Water AN 819

Organochlorine Pesticides GC-ECD Drinking Water AN 1004

Sex Hormones HPLC-UV Drinking Water TN 148

Tricolsan HPLC-UV Drinking Water AN 1081

Explosives HPLC-UV Ground Water AN 358

Linear Alkyl Benzene Sulfonate HPLC-UV Waste Water AN 1080

Organophosphorous Pesticides GC-NPD Drinking Water Pending Publication

Visit thermoscientific.com/samplepreparation

Key Applications Summary

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U.S. EPA SPE 500 Methods

EPA Method Analytes Extraction and Analytical Methods Chemistry Used

506 Phthalate and Adipate Esters SPE and GC/PID C18

507 N and P containing Pesticides SPE and GC C18

508.1 Chlorinated pesticides, herbicides and organohalides SPE and GC-ECD C18

521 Nitrosamines SPE and GC/MS/MS Carbon

522 Dioxane SPE and GC/MS Carbon

525.2 Semivolatile Organic Compounds (SVOC) SPE and GC/MS C18

525.3 Semivolatile Organic mpounds (SVOC) SPE and GC/MS C18

526 Semivolatile Organic in DW SPE and GC/MS HRPHS

527 Flame Retardants SPE and GC/MS HRPHS

528 Phenols SPE and GC/MS HRPHS

529 Explosives SPE and GC/MS HRPHS

532 Phenylurea SPE and HPLC C18

535 Acetic Herbicides SPE and LC/MS/MS Graphitized carbon

548 Endothal SPE and GC/ECD C18

539 Hormones SPE and LC/MS/MS HRPHS

553 Benzidines and N containing Pesticides SPE and LC/MS C18

554 Carbonyl compounds SPE and LC C18

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U.S. EPA SPE 600 /1600 Methods

EPA Method Analytes Extraction and Analytical Methods Chemistry Used

606,608, 609, 611, 612 Organochlorine Pesticides and PCB’s SPE and GC/ECD C18

1613 Dioxins and Furans SPE and GC/MS C18

1614 Brominated Diphenyl Ehters SPE and HRGCMS C18

1657 Organophosphorous Pesticides GPC/SPE and GC C18

1668a PCB and congeners SPE and HRGC/HRMS C18

1694 Pharmaceuticals & Personal Care Products SPE and LC/MS/MS HRPHS