Extraction of Phthalates from Solid and Liquid Matrices

Transcription

1 Extraction of s from Solid and Liquid Matrices David E. Knowles, Brian C. Dorich, Richard E. Carlson, Brett J. Murphy, Eric S. Francis, Jennifer Paterson, and Bruce E. Richter; Thermo Fisher Scientific, Sunnyvale, California

2 Introduction FIGURE 2. Dionex ASE 150 a s are a group of chemicals used primarily in the consumer product industry. One of their main uses is as a softener in PVC plastic for a wide range of products everything from toys to footwear. They are also used in cosmetics, perfume, and pharmaceutical packaging. When used in PVC production, phthalates do not chemically bind to the PVC, but tend to evaporate into the air and leach into water and soil over time. In this way, humans and other living organisms are exposed to these toxic phthalates through direct contact with contaminated food, water, and air. Therefore, some phthalate compounds are classified as toxic to reproduction and can cause reduced fertility and/or potential harm to the unborn child. Sample Extraction Issues Sample handling is the primary source of errors Sample extraction causes the biggest bottleneck for most analysis methods Costs are increasing for solvent purchase and disposal The data is only as good as the sample preparation High-price chromatography and data systems do not improve the quality of data from poorly prepared samples The Thermo Scientific Dionex ASE Accelerated Extractor and Thermo Scientific Dionex AutoTrace 280 Solid-Phase Extraction instrument address these issues. Overview of Automated Extraction The automated solvent extraction technique uses liquid solvents and solvent mixtures to extract solid or semisolid samples. This method uses elevated temperatures (0 200 C) and pressure ( psi) to accelerate the extraction process. Smart Run System Detects Cell Size Fill, Heat, and Pressurize Static Extraction Cycle Flush with Fresh Purge with Nitrogen Pump 0. Mixing Relief Pretreated Matrix In-Cell Clean Up Oven Chemistry Extraction 1 2 min Static Extract Ready 2 Extraction of s from Solid and Liquid Matrices Total 12 1 min Sample Preparation Shoes were cut into pieces an Extraction Conditions FIGURE 1. Automated solvent extraction schematic Extraction of Pl System Collection Bottle Pressure: 1500 ps Oven Temperature: 120 C Heat Time: Static Time: 2 5m Flush Volume: 60% of Purge Time: 60 s : Hexane

3 FIGURE 2. Dionex ASE 150 and 50 Accelerated Extractors Table 1. Results for Plastic Shoes Sample the consumer product industry. for a wide range of products n cosmetics, perfume, and mically bind to the PVC, but tend over time. In this way, humans phthalates through direct contact me phthalate compounds are uced fertility and/or potential harm for most analysis methods Country of Purchase DB sposal on ms do not improve the quality of olvent Extractor and Thermo raction instrument address these lvent Extraction id solvents and solvent mixtures to elevated temperatures ate the extraction process. Extraction of Plastic Shoes Using the ASE System Sample Preparation Shoes were cut into pieces and put into 10 ml cells. Extraction Conditions ic Mixing Relief Pressure: 1500 psi (6.89 MPa) Oven Temperature: 120 C Heat Time: Static Time: 2 cycles Flush Volume: 60% of cell volume Purge Time: 60 s : Hexane Overview of the Di Solid-Phase Extrac Automates sample preparation (SPE) Processes one to six samples Sample volumes of 20 ml to Uses normal or reverse-phase c Accepts 1,, and 6 ml cartridge Saves time and reduces costs Automatically loads and elutes S Unattended operation Uses positive pressure to load a Oven Provides constant, reproducib Chemistry Extraction Independently controls flow fo No hood is requiredclosed Static Collection Bottle Thermo Scientific Poster Note PN7089_E 11/1S

4 ted Extractors Table 1. Results for Plastic Shoes1 Sample Country of Purchase DBP DEHP BBP DnOP DINP DIDP % % 9.60% 0.90%.70% 0.81% 12.70% % 6.70% 6 2.2% 7 0.2% 6.80% 8 1% 7.20% 2% 1.20% %.60% 10.80% 19.0% 11.0%.20% % 0.6% 1 7.0% 5.00% 1 2% 18.60% % 18.10% 7.90% 7% 17 % 15.80% EPA Method 625 AutoTrace 280 S Instrument Sample Pretreatment oes Using the ASE cells. FIGURE. Dionex AutoTrace configuration (left) and disk Add 2.5 ml of methanol and 2 Overview of the Dionex AutoTrace 280 Solid-Phase Extraction Instrument Condition, Rinse, and Load P (Thermo Scientific Dionex Rinse cartridge with 2 ml Automates sample preparation for liquid samples using solid-phase extraction (SPE) Rinse cartridge with 5 ml Processes one to six samples Load 550 ml of sample o Sample volumes of 20 ml to 20L Uses normal or reverse-phase cartridges and disks Condition cartridge with 1 Dry cartridge with gas for Sample Elute Program Accepts 1,, and 6 ml cartridges and disks Collect 5 ml fraction using Saves time and reduces costs Collect 2 ml fraction using Automatically loads and elutes SPE cartridges/disks Unattended operation Uses positive pressure to load and elute samples SPE Parameters s 1: Water (reagent Provides constant, reproducible flow of liquids 2: Methanol Independently controls flow for each channel : Ethyl acetate No hood is requiredclosed system with fan to vent solvent vapors : Methylene chlo Flow Rates Load flow: ml/min Rinse flow: 0 ml/min Elute flow: 20 ml/min Rinse, air push: 20 ml/mi Sample is Now Ready for An Evaporation Analysis using gas chrom Extraction of s from Solid and Liquid Matrices

5 BBP DnOP DINP DIDP FIGURE. Dionex AutoTrace 280 Solid-Phase Extraction instrument cartridge configuration (left) and disk configuration (right) Tables 2 and show GC/MS results Dionex AutoTrace 280 instrument. Table 2. River Water Sample #1.70% Class (n=).60% 19.0%.20% Table. River Water Sample #2 Class (n=) EPA Method 625 Using the Dionex AutoTrace 280 Solid-Phase Extraction Instrument Sample Pretreatment Add 2.5 ml of methanol and 2 ml of concentrated sulfuric acid to 500 ml of sample. using solid-phase extraction o vent solvent vapors Number of Com sks ks Data all fall within acceptable limits for EPA 1.20% otrace 280 rument Number of Com Condition, Rinse, and Load Program (Thermo Scientific Dionex SolEx SPE cartridges C18, 6 ml) Rinse cartridge with 2 ml of methanol Rinse cartridge with 5 ml of EtOAc and DCM Condition cartridge with 10 ml of CHOH and water Load 550 ml of sample onto cartridge Dry cartridge with gas for 10 min Sample Elute Program Conclusion Extraction of phthalates from liquid o using automated sample preparation Accelerated Extractor system samples quickly and effectively, usin be extracted automatically from wate Solid-Phase Extraction instrument. T powerful tools to decrease sample p while cutting solvent costs. Reference 1. Swedish Society for Nature Co from all over the world. Report engelska/chemicals_in_plastic_ Collect 5 ml fraction using EtOAc Collect 2 ml fraction using DCM SPE Parameters s 1: Water (reagent grade) 2: Methanol : Ethyl acetate : Methylene chloride Flow Rates Load flow: ml/min Rinse flow: 0 ml/min Elute flow: 20 ml/min Rinse, air push: 20 ml/min Sample is Now Ready for Analysis Evaporation Analysis using gas chromatography/mass spectrometry (GC/MS) All trademarks are the property of Thermo Fish This information is not intended to encourage u intellectual property rights of others. Thermo Scientific Poster Note PN7089_E 11/1S 5

6 se Extraction instrument cartridge right) Tables 2 and show GC/MS results of two river water samples prepared with the Dionex AutoTrace 280 instrument. Table 2. River Water Sample #1 Class (n=) Number of Compounds Range RSD% 68% 10%.0% 8.% 6% 9% 5.0% 1.0% 85% 95%.0% 1.6% Data all fall within acceptable limits for EPA Method 625 Table. River Water Sample #2 Class (n=) Number of Compounds the Dionex ase Extraction ted sulfuric acid to 500 ml of sample. artridges C18, 6 ml) Range RSD% 60.6% 99.2%.7% 8.8% 5.2% 79.0% 2.6% 1.% 7.7% 81.9% 1.5% 6.9% Conclusion Extraction of phthalates from liquid or solid samples can be made easier and faster by using automated sample preparation systems. The data shows that the Dionex ASE Accelerated Extractor system can automatically extract phthalates from solid samples quickly and effectively, using minimal amounts of solvent. s can also be extracted automatically from water samples by using the Dionex AutoTrace 280 Solid-Phase Extraction instrument. These two extraction systems offer laboratories powerful tools to decrease sample preparation bottlenecks and increase productivity, while cutting solvent costs. Reference CM and water 1. Swedish Society for Nature Conservation. Chemicals up close: Plastic shoes from all over the world. Report [Online], engelska/chemicals_in_plastic_shoes.pdf (accessed Feb 22, 2011). spectrometry (GC/MS) All trademarks are the property of Thermo Fisher Scientific and its subsidiaries. This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others. 6 Extraction of s from Solid and Liquid Matrices

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