2010 10 October 2010 ROCK AND MINERAL ANALYSIS Vol. 29 No. 5 503 ~ 507 0254 5357 2010 05 0503 05-1 2 3 1 1 1. 100037 2. 710021 3. 100083 13 Carb Rtx - OPP2-0. 67 ~ 1. 50 ng /ml 0. 67 ~ 600 ng /ml 0. 999 4 ~ 0. 999 9 54. 3% ~ 106% 60. 7% ~ 133% RSD n = 5 2. 2% ~ 9. 9% O652. 62 O657. 71 S151. 93 S482. 33 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 100037 China 2. Oil & Gas Technology Research Institute of Ghangqing Oilfield Company Xi'an 710021 China 3. Civil and Environmental Engineering College University of Science and Technology Beijing 100083 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 0. 67 ~ 1. 50 ng /ml with linear ranges of 0. 67 ~ 600 ng /ml and correlation coefficients of 0. 999 4 ~ 0. 999 9. 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 2010-01-18 2010-07-22 200120190107-05 1212010816028-02 1212010634607 1962 - E-mail raozhu@ 126. com 503
http www. ykcs. ac. cn 2010 OPPs 1-8 OPPs Supelco OPPs 1. 3 OPPs - 9 OPPs 1 1 70 10. 5 MPa 5 min 5 min 3 10-13 1. 4 ASE 1996 DIONEX 200 5. 0 min 10 /min ASE 250 220 280 14 3. 0 ml /min 4. 0 ASE 12 ~20 min μl 34. 4 kpa 82. 0 ml /min 15 15 ~ 45 ml -17 90. 0 ml /min ASE - GC - FPD 1. 5 OPPs 600 12 h 0. 175 mm OPPs 1. 6 13 OPPs ASE OPPs 10 d OPPs 1. 7 1. 7. 1 Supelclean ENVI - Carb 120 10 /min 10. 00 g 4. 00 g 1 22 ml ASE 1. 1 OPPs GC - 2010 1. 3 ASE FPD 1. 0 ml Rtx - OPP2 30. 0 m 1. 7. 2 0. 53 mm 0. 5 μm RESTEK 10 ml ENVI - Carb ASE 200 DIONEX ENVI - Carb 25 ml - 2 1 4 500 mg /6 ml ml /min 1. 2 1. 00 ml 13 OPPs 1. 8 GC - MS OPPs 504
- 29 2. 3 65% ~130% OPPs 2 2. 1 R 2 0. 9995 ~ 0. 9990 OPPs 5 1 OPPs - 1 1 - OPPs OPPs 70 2 3 OPPs 1 13 Fig. 1 Chromatogram of 13 organophosphate 2. 2 SPE 1 2 3 4 5 6 7 8 9 10 11 12 13 SPE C 18 Al 2 O 3 Carb 18 - SAX /NH 19 2 OPPs Carb 2. 4-1 1 - ENVI - Carb 5 1 2 13 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 /% 30. 0 26. 3 87. 5 12. 5 30. 0 28. 0 93. 3 6. 7 30. 0 28. 7 95. 6 4. 4 30. 0 25. 6 85. 3 14. 7 30. 0 28. 1 93. 8 6. 2 30. 0 30. 9 103 3. 0 30. 0 31. 5 105 5. 0 30. 0 27. 5 91. 8 8. 2 30. 0 26. 5 88. 2 11. 8 30. 0 29. 5 98. 2 1. 8 30. 0 27. 6 92. 0 8. 0 30. 0 26. 8 89. 2 10. 8 30. 0 23. 9 79. 8 20. 2 1 n = 3 0. 67 ~ 1. 50 ng /ml 13 OPPs 1. 2 ~ 600 ng /ml 2 pesticides in standard sample 3 10. 00 g 3 2 OPPs OPPs 2 3 2 54. 3% 90% 505
http www. ykcs. ac. cn 2010 74. 4% 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 /% 1. 50 3. 0 ~ 600. 0 78. 4 2. 6 0. 87 1. 3 ~ 260. 0 98. 7 8. 6 0. 67 2. 0 ~ 400. 0 89. 0 8. 6 1. 00 1. 5 ~ 300. 0 87. 6 9. 7 1. 00 1. 5 ~ 300. 0 106 3. 6 0. 80 1. 2 ~ 240. 0 89. 0 7. 9 0. 86 1. 5 ~ 300. 0 94. 6 7. 8 1. 44 1. 8 ~ 360. 0 60. 7 2. 2 1. 31 2. 3 ~ 460. 0 81. 0 3. 7 0. 86 1. 5 ~ 300. 0 92. 4 9. 9 1. 15 2. 3 ~ 460. 0 79. 4 5. 2 1. 42 2. 5 ~ 500. 0 82. 0 5. 3 1. 43 2. 5 ~ 500. 0 54. 3 6. 0 S. 3 13 2. - 1 J. 2008 27 Table 3 Analytical results of OPPs and average recoveries 1 12-16. 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 0. 41 0. 36 0. 63 0. 42 91. 8 92. 8 2003 51 24 6915-6921. - - - - 96. 1 93. 9 4 Ahmad N Bugueno G Guo L Marolt R. Determination - - - - 83. 8 85. 6 of organochlorine and organophosphate pesticide 0. 17 0. 30 0. 91 0. 54 97. 3 95. 1 residues in fruits vegetables and sediments J. - - - - 117 125 Journal of Environment Science and Health Part B - - - - 74. 4 113 1999 34 5 829-848. - 0. 79-0. 20 84. 5 73. 5 5. 15 - - - - 79. 6 60. 7 J. 2007 26 1 17-20. - - 0. 35 0. 22 69. 9 88. 4 0. 65 117 306 38. 3 71. 6 95. 8-0. 21 0. 94-71. 2 76. 1 - - - - 133 108 - - - - 91. 6 99. 7 1 - of Science & Technology 2003 11 1 93-105. 4 8 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 506 2 Fig. 2 Chromatogram of OPPs in soil sample collected from peach garden 1 2 3 4 5 6 13 5 1 GB /T 5009. 1992003 6 A rapid method for trace organophosphorus pesticides in drinking water EB /OL. http www. chem. agilent. com / Library / applications /5990-3158EN. 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
- 29 detection J. Journal of Chromatography B Biomedical Sciences and Applications 2001 759 1 109-116. 9 Sattar M A. Fate of organophosphorus pesticides in soils J. Chemosphere 1990 20 3-4 387-396. 10. GC - MS J. 2007 31 2 27-28. 11 GB /T 145522003 18 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. 1998. 13. Acta 2001 444 1 87-95. J. 2007 36 2 212-214. 14 US EPA Method 3545 Pressurized fluid extraction PFE S. 15. - J. 2005 33 6 821-824. 16. - J. 2008 17 6 46-48. 17 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. 2005 26 29 299-302. 20. J. 2009 28 12 1368-1372 1377. CN11-2017 /TF 82-431 CODEN FENSE4 M848 ISSN 1000-0720 0038 16 128 1982 CA 2011 18 12 216 82-431 2 100088 010-82013328 E - mail analysislab@ 263. net ana - info@ 263. net 507