Determination of Organophosphate Pesticides in Soil Samples by Accelerated Solvent Extraction-Gas Chromatography

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1 October 2010 ROCK AND MINERAL ANALYSIS Vol. 29 No ~ Carb Rtx - OPP ~ ng /ml ~ 600 ng /ml ~ % ~ 106% 60. 7% ~ 133% RSD n = % ~ 9. 9% O O S S A Determination of Organophosphate Pesticides in Soil Samples by Accelerated Solvent Extraction-Gas Chromatography RAO Zhu 1 HE Miao 2 CHEN Wei 3 LI Song 1 LIU Yan 1 1. National Research Center for Geoanalysis Beijing China 2. Oil & Gas Technology Research Institute of Ghangqing Oilfield Company Xi'an China 3. Civil and Environmental Engineering College University of Science and Technology Beijing China Abstract A method for the determination of organophosphate pesticides OPPs in soil samples by accelerated solvent extraction-gas chromatography ASE-GC was developed. Through the extraction by ASE clean-up with Carb column 13 OPPs in soil samples were separated and determined by Rtx-OPP2 wide bore capillary-gas chromatography with electron capture detector. The detection limits of the method for OPPs were ~ ng /ml with linear ranges of ~ 600 ng /ml and correlation coefficients of ~ The average recoveries for 13 OPPs in simulated soil samples and real soil samples were 54. 3% ~ 106% and 60. 7% ~ 133% with precision of 2. 2% ~ 9. 9% RSD n = 5. The method provides the advantages of high sensitivity high reliability convenience and is suitable for analysis of OPPs in soil samples. Key words accelerated solvent extraction gas chromatography organophosphate pesticides soil OPPs OPPs OPPs OPPs raozhu@ 126. com 503

2 http www. ykcs. ac. cn 2010 OPPs 1-8 OPPs Supelco OPPs 1. 3 OPPs - 9 OPPs MPa 5 min 5 min ASE 1996 DIONEX min 10 /min ASE ml /min 4. 0 ASE 12 ~20 min μl kpa ml /min ~ 45 ml ml /min ASE - GC - FPD 1. 5 OPPs h mm OPPs OPPs ASE OPPs 10 d OPPs Supelclean ENVI - Carb /min g g 1 22 ml ASE 1. 1 OPPs GC ASE FPD 1. 0 ml Rtx - OPP m mm 0. 5 μm RESTEK 10 ml ENVI - Carb ASE 200 DIONEX ENVI - Carb 25 ml mg /6 ml ml /min ml 13 OPPs 1. 8 GC - MS OPPs 504

3 % ~130% OPPs R ~ OPPs 5 1 OPPs OPPs OPPs OPPs 1 13 Fig. 1 Chromatogram of 13 organophosphate 2. 2 SPE SPE C 18 Al 2 O 3 Carb 18 - SAX /NH 19 2 OPPs Carb ENVI - Carb OPPs 54. 3% 1 1 ENVI - Carb 60. 0% ~ 106% RSD n = 5 Table 1 The average recoveries of organophosphate pesticides with ENVI-Carb column 2. 2% ~ 9. 9% m /ng R /% RSD /% n = ~ ng /ml 13 OPPs 1. 2 ~ 600 ng /ml 2 pesticides in standard sample g 3 2 OPPs OPPs % 90% 505

4 http www. ykcs. ac. cn % 113% 38. 6% 20 2 Table 2 The average recoveries of OPPs in synthesized soil samples and performance of the method L D/ ng ml - 1 ρ B / ng ml - 1 R /% RSD /% ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ S J Table 3 Analytical results of OPPs and average recoveries of OPPs in practical samples 3 Albero B Sánchez-Brunete C Tadeo J L. Determination w OPPs / ng g - 1 R /% 50 ng of organophosphorus pesticides in fruit juices by matrix solid-phase dispersion and gas chromatography J. Journal of Agricultural and Food Chemistry Ahmad N Bugueno G Guo L Marolt R. Determination of organochlorine and organophosphate pesticide residues in fruits vegetables and sediments J Journal of Environment Science and Health Part B J of Science & Technology Lacassie E Dreyfuss M F Gaulier J M Marquet P Daguet J L Lachatre G. Multiresidue determination Rtx - OPP2 method for organophosphorus pesticides in serum and - - whole blood by gas chromatography-mass-selective Fig. 2 Chromatogram of OPPs in soil sample collected from peach garden GB /T A rapid method for trace organophosphorus pesticides in drinking water EB /OL. http www. chem. agilent. com / Library / applications / EN. pdf. 7 Chai A L K Lau S. Determination of organophosphorous pesticid in vegetables by solid-phase extraction cleanup and gas chromatography J. Pertanika Journal

5 - 29 detection J. Journal of Chromatography B Biomedical Sciences and Applications Sattar M A. Fate of organophosphorus pesticides in soils J. Chemosphere GC - MS J GB /T Chuang J C Hart K Chang J S Boman L E Van S. Emon J M Reed A W. Evaluation of analytical 12 EPA Method 8141B Gas chromatographic analysis of methods for determining pesticides in baby foods and organophosphate compounds S Acta J US EPA Method 3545 Pressurized fluid extraction PFE S J J Extraction of organophosphorus pesticides from soils by pressurized solvent extraction EB /OL. http www. appliedseparations. pse203. pdf. com/ Applications/ downloads/ onepse/ adult duplicate-diet samples J. Analytica Chimica 19. J J CN /TF CODEN FENSE4 M848 ISSN CA E - mail analysislab@ 263. net ana - info@ 263. net 507

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