环境水中Dichlorvos检测方案(固相萃取仪)

SCIENTIFICPart of Thermo Fisher Scientific EPA Method 525.2： Extraction ofSemivolatile Organic Compoundsfrom Water Using AutoTrace 280Solid-Phase Extraction Cartridges Introduction Traditionally， semivolatiles in drinking water have beenextracted using liquid-liquid extraction techniques such asseparatory funnel or continuous liquid-liquid extraction.While these techniques are effective， they use largevolumes of organic solvent (up to 300 mL per sample)and require extensive user intervention or monitoring.Solid-phase extraction (SPE) is an alternative acceptedextraction technique for USEPA Method 525.2 whichuses significantly less solvent (up to 60 mL per sample).The Thermo Scientific Dionex AutoTrace 280 extractioninstument offers an automated SPE technique that savessolvent and time， and decreases user intervention thanksto automation. With the Dionex AutoTrace 280" system， the compoundsof interest are trapped on SPE adsorbents， then elutedwith liquid solvents to generate an extract that is readyfor analysis. The Dionex AutoTrace 280 system savestime， solvent， and labor ensuring high reproducibilityand productivity for analytical laboratories. The unitcan process up to six samples with minimal operatorinvolvement. The Dionex AutoTrace 280 system usespowerful pumps (no check valves) and a proven positive-pressure technology to efficiently process liquid samples.Current analytical methods that may require SPE samplepreparation include GC， GC-MS， LC， and LC-MS. This work describes the use of the Dionex AutoTrace 280instrument for extraction of semivolatile organic compoundsfrom water samples. Equipment Dionex AutoTrace 280 Automated Large Volume SPEinstrument for 6 mL Cartridges (Thermo ScientificPN071385) 15 mL Conical Tubes (pack of 12) (Thermo ScientificPN 071056) Required Solvents Ethyl acetate (EtOAc) Methylene chloride (CH，Cl，) Methanol (MeOH) Water Standards Restek (#31899) Semivolatiles Mix Restek (#32415) OCP Mix AB #3 Restek (#33011) 525.2 Revised Chlorinated Pesticides Mix #2 Restek (#564292) Custom 525.2 Pesticide Std. Restek (#565293) Custom 525.2 Misc Std. Restek (#31825) Method 525.2 Internal Std MixRestek (#31826) Surrogate Mix Solvent Bottle No. Solvent Type 1 Water 2 MeOH 3 1：1 CH，CI，：Et0Ac 4 CH，CI 5 Et0Ac 525.2 Solid-Phase Extraction Method Enter the following method into the Dionex AutoTrace 280 program： No. Method User Intervention 1 Process 6 samples using the following method steps 2 Rinse Cartridge with 5.0 mL of Et0Ac into Solvent Waste 3 Rinse Cartridge with 5.0 mL of CH，CI， into Solvent Waste 4 Condition Cartridge with 10.0 mL of Me0H into Solvent Waste 5 Condition Cartridge with 10.0 mL of Water into Aqueous Waste 6 Load 1100.0mL of Sample onto Cartridge 7 Pause and Alert operator， resume when CONTinue is pressed - Check sample bottle to ensure all sample has been removed.-Add 5 mL Et0Ac to each sample bottle and swirl to coat all sides of bottle.- Let stand. 8 Load 60.0 mL of Sample onto Cartridge 9 Dry Cartridge with gas for 10.0 minutes 10 Wash Syringe with 5.0 mL of Me0H 11 Soak and Collect 4.0 mL Fraction using Et0Ac 12 Pause for 2.0 minutes 13 Soak and Collect 4.0 mL Fraction using 1：1 CH，CI，：Et0Ac 14 Pause for 2.0minutes 15 Collect 4.0 mL Fraction into collection vial using CH，CI， 16 Collect 4.0 mL Fraction into collection vial using CH，CI， 17 End Save and download this program on the Dionex AutoTrace 280 system for future use. Note： Up to 24 different programscan be saved onto the system. These methods can be written and transferred to the Dionex AutoTrace system viacomputer. Once the desired methods are stored on the Dionex AutoTrace 280 instrument， there is no further need for itto be connected to the computer. Enter the following parameters for the Solid-Phase Extract under the Params Tab： Flow Rates SPE Parameters Cond Flow 40 mL/min Push Delay 5 sec Load Flow 20 mL/min Air Factor 1.0 Rinse Flow 40 mL/min Autowash Vol. 2.00 mL Elute Flow 5 mL/min Instrument Parameters Cond Air Push 15 mL/min Max. Elution Vol. 16.0 mL Rinse Air Push 20 mL/min Exhaust Fan Yes Elute Air Push 5 mL/min Beeper On Yes It is advisable to clean the sample path after each batch of samples. The following is a suggested method that can be used： No. Method User Intervention 1 Process 6 samples using the following method steps 2 Clean Sample Path with 25 mL Et0Ac into Solvent Waste Place sample lines in Et0Ac 3 Clean Sample Path with 25 mL Me0H into Solvent Waste Place sample lines in MeOH 4 Clean Sample Path with 25 mL Water into Solvent Waste Place sample lines in Water 5 Dry Cartridge with gas for 10.0 minutes 6 End Results and Discussion Pour the extracts through glass funnels containing a filter and 5-7 g of heat-treated sodium sulfate. Remove thesample bottles from the Dionex AutoTrace 280 instrument and pour the EtOAc that was used to rinse these bottles throughthe corresponding funnel containing sodium sulfate. Add 5 mL CH，Cl to each sample bottle and swirl. Pour this throughthe corresponding funnel containing sodium sulfate. Concentrate the final sample extracts to 1 mL. Analyze by GC/MS. The results listed in Table 1 show recoveries of semivolatile organic compounds from 4 spiked samples that wereextracted using the AutoTrace 280 system. Ethyl-Parathion 1.000 1.028 102.8 Table 1. Recoveries of OCPs from water using the Dionex AutoTrace 280 system. Conclusions .The Dionex AutoTrace 280 instrument with thecartridge configuration provides an automated， solid-phase extraction system that replaces traditional liquid-liquid extraction. Results show that using the cartridgeconfiguration gives excellent recovery and precision results. Thanks to Beau Sullivan at the Santa Clara Valley WaterDistrict for providing the data used. List of Manufacturers Thermo Fisher Scientific， 2000 Park Lane，Pittsburgh， PA 15275-1126 USA， Tel： 800-766-7000，www.fishersci.com.Restek， 110 Benner Circle， Bellefonte， PA 16823 USA，Tel：800-356-1688www.restek.com ( Legal Notices： O2011 T h ermo Fisher Scien t ific Inc. All rights res e rved. 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Dionex Products：(408)737-0700 North America： U.S./Canada (847)295-7500 South America： Brazil (55) 11 3731 5140 Europe： Austria (43)616 51 25 Benelux (31)20 683 9768 (32)3353 4294 Denmark (45) 36 36 90 90 France (33) 1 39 30 01 10 Germany (49)61125991 0 Ireland (353)644 0064 Italy (39) 02 51 62 1267 Sweden (46)8 473 3380 Switzerland (41) 62 205 9966 United Kingdom(44) 1276691722Asia Pacific：Australia(61)29420 5233China(852) 2428 3282India (91) 2227642735Japan(81) 6885 1213Korea(82)22653 2580Singapore(65)6289 1190Taiwan (886)2875 6655 AN819_E11/11SVLPN3025 Traditionally, semivolatiles in drinking water have been extracted using liquid-liquid extraction techniques such as separatory funnel or continuous liquid-liquid extraction. While these techniques are effective, they use large volumes of organic solvent (up to 300 mL per sample) and require extensive user intervention or monitoring.Solid-phase extraction (SPE) is an alternative accepted extraction technique for USEPA Method 525.2 which uses significantly less solvent (up to 60 mL per sample).The Thermo Scientific Dionex AutoTrace 280 extraction instument offers an automated SPE technique that saves solvent and time, and decreases user intervention thanksto automation.With the Dionex AutoTrace 280™ system, the compounds of interest are trapped on SPE adsorbents, then eluted with liquid solvents to generate an extract that is ready for analysis. The Dionex AutoTrace 280 system saves time, solvent, and labor ensuring high reproducibility and productivity for analytical laboratories. The unit can process up to six samples with minimal operator involvement. The Dionex AutoTrace 280 system uses powerful pumps (no check valves) and a proven positivepressure technology to efficiently process liquid samples.Current analytical methods that may require SPE sample preparation include GC, GC-MS, LC, and LC-MS. This work describes the use of the Dionex AutoTrace 280 instrument for extraction of semivolatile organic compounds from water samples.