Multiresidue Method for Determination of Organophosphorous Pesticide Residues in Animal Origin Foods by Gas Chromatograph - Flame Photometric Detector (GC-FPD)
Abstract
A rapid and simple multiresidue method has been developed and validated for determination of organophosphorous (OP) pesticide residues in animal origin foods by gas chromatograph - flame photometric detector (GC-FPD). The pesticides were extracted from food product samples with acetonitrile and homogenized by using a shaker. Dichloromethane (CH2Cl2) and sodium chloride (NaCl) were added to the extract followed by filtration to remove solid residue. Water residue in the filtrate layer was removed by adding anhydrous sodium sulfate (Na2SO4). After removal of the solvent, the residue was dissolved to reconstitute in acetone. The final extract of test solution was subjected to GC-FPD. Recovery tests of 22 pesticides in three kinds of foods; dried fish, fermented fish and fried crickets were performed at three different fortification levels of 0.1, 0.5 and 1 mg/kg and 13 pesticides showed acceptable recoveries (60-120%) and repeatability (HORRAT<2). The limit of detection (LOD) and the limit of quantitation (LOQ) of the method are 0.03 and 0.1 mg/kg, respectively. The developed method was applied to determine OP pesticides in real samples. One hundred and thirty-three food samples were analyzed during 2011 to 2015. Residual trichlorfon was detected at <0.01-34.1 mg/kg in 32 samples of dried fish (24%). These results indicated that the problem of miss used trichlorfon still exists. The relevant authorities should be concerned to solve systematically the problem.Keywords: Multiresidue analysis, Organophosphorous pesticide, Animal origin food, Gas chromatographyReferences
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Atisook, K. (2010). Surveillance of pesticide residues in fermented fish. News Letter of the Department of Medical Sciences, 24(7), 11. (in Thai)
Bentabol, A. & Jodral, M. (1995). Determination of organochlorine pesticides in cheese. Journal of the Association of Official Analytical Chemists, 78, 94D98.
Catalgol, B.K., Ozden, S. & Alpertunga, B. (2007). Effects of trichlorfon on malondialdehyde and antioxidant system in human erythrocytes. Toxicology in Vitro, 2, 1538-1544.
Codex Alimentarius Commission. (2011). CAC/GL 59-2006 (Amendment 1-2011) Guidelines on Estimation of Uncertainty of Results. Retried January 15, 2016, from www.codexalimentarius.net/download/standards/10692/cxg_059e.pdf
Ellison, S.L.R., Rosslein, M., & Williams, A. (2000). EURACHEM Guide: Quantifying Uncertainty in Analytical Measurements, Laboratory of the Government Chemist, 2nd edition, London.
Eurolab Technical Report. (2007). Measurement uncertainty revised: alternative approaches to uncertainty evaluation, European Federation of National Associations of Measurement, Testing and Analytical Laboratories. Retried January 15, 2016, from www.eurolab.org
Guimarães, A.T.B., Silva de Assis, H.C. & Boeger, W. (2007). The effect of trichlorfon on acetycholinesterase activity and his- topathology of cultivated fish Oreochromis niloticus. Ecotoxicology and Environmental Safety, 68, 57-62.
Harnpicharnchai, K., Chaiear, N. & Charerntanyarak, L. (2013). Residues of organophosphate pesticides used in vegetable cultivation in ambient air, surface water and soil in Bueng Niam Subdistrict, Khon Kean Thailand. The Southeast Asian Journal of Tropical Medicine and Public Health, 44, 1088-1097.
Khay, S., Abd El-Aty, A.M., Choi, J.H., Shin, E.H., Shin, C.H., Chang, B.J., Lee, C.H., Shin, S.C., Jeong, J.Y. & Shim, J.H. (2009). Simultaneous determination of pyrethroids from pesticide residues in porcine muscle and pasteurized using GC. Journal of Separation Science, 32, 244-251.
Lehotay, S.J., Lightfield, A.R., Harman-Fetcho, J.A. & Donoghue, D.J. (2001). Analysis of pesticide residues in eggs by direct sample introduction/gas chromatography/tandem mass spectrometry. Journal of Agricultural and Food Chemistry, 49, 4589-4596.
Lertruengdej, Y. & Chongmevasna, P. (1997). Analysis of Trichlorfon in Dry Salted Fish. Bulletin of the Department of Medical Sciences, 39(1), 45-51. (in Thai)
Malone, E.M., Elliott, C.T., Kennedy, D.G.& Regan, L. (2010). Rapid confirmatory method for the determination of sixteen synthetic growth promoters and bisphenol A in bovine milk using dispersive solid-phase extraction and liquid chromatographytandem mass spectrometry. Journal of Chromatography B, 878, 1077- 1084.
Ngoh, M.A. & Cullison, R. (1996). Determination of trichlorfon and dichlorvos residues in shrimp using gas chromatography with nitrogen-phosphorus detection. Journal of Agricultural and Food Chemistry, 44, 2686-2689.
Nordtest, R. (2004). Handbook for Calculation of Measurement Uncertainty in Environmental Laboratories. Retried January 15, 2016, from http://www.nordicinnovation.net/nordtestfiler/tec537.pdf
Park, J.W., Abd El-Aty, A.M., Lee, M.H., Song, S.O. & Shim, J.H. (2006). Residue Analysis of organophosphorus and organochlorine pesticides in fatty matrices by gas chromatography coupled with electron-capture detection. Zeitschrift für Naturforschung, 61c: 341D346.
Pico, Y., Font, G., Molto, J.C. & Manes, J. (2000). Pesticide residue determination in fruit and vegetables by liquid chromatography-mass spectrometry. Journal of Chromatography A, 16, 153D173.
SANCO. (2012). European Commission Health & Consumer Protection Directorate-Gener. Safety of the food chain Chemicals, contaminants, pesticides. Retried January 15, 2016, from http://ec.europa.eu/food/plant/pesticides/guidance_documents/docs/qualcontrol_en.pdf
Sultatos, L.G. (1994). Mammalian toxicology of organophosphorus pesticides. Journal of Toxicology and Environmental Health, Part A, 43, 271D289.
Thoophom, G., Sungvaranond, B., Atisook K., Lertruengdej, Y., Kaewklapanyachareon, L., Suntudrob, J., Chongmevasna, P. & Boonthai, R. (1995). Pesticide and PCB Residues in Foods, 1991-1993. Bulletin of the Department of Medical Sciences, 37(2), 145-160. (in Thai)
Zrostlíkovµ, J., Lehotay, S.J.& HajsÏlovµ, J. (2002). Simultaneous analysis of organophosphorus and organochlorine pesticides in animal fat by gas chromatography with pulsed flame photometric and micro-electron capture detectors. Journal of Separation Science, 25, 527-537.
Atisook, K. (2010). Surveillance of pesticide residues in fermented fish. News Letter of the Department of Medical Sciences, 24(7), 11. (in Thai)
Bentabol, A. & Jodral, M. (1995). Determination of organochlorine pesticides in cheese. Journal of the Association of Official Analytical Chemists, 78, 94D98.
Catalgol, B.K., Ozden, S. & Alpertunga, B. (2007). Effects of trichlorfon on malondialdehyde and antioxidant system in human erythrocytes. Toxicology in Vitro, 2, 1538-1544.
Codex Alimentarius Commission. (2011). CAC/GL 59-2006 (Amendment 1-2011) Guidelines on Estimation of Uncertainty of Results. Retried January 15, 2016, from www.codexalimentarius.net/download/standards/10692/cxg_059e.pdf
Ellison, S.L.R., Rosslein, M., & Williams, A. (2000). EURACHEM Guide: Quantifying Uncertainty in Analytical Measurements, Laboratory of the Government Chemist, 2nd edition, London.
Eurolab Technical Report. (2007). Measurement uncertainty revised: alternative approaches to uncertainty evaluation, European Federation of National Associations of Measurement, Testing and Analytical Laboratories. Retried January 15, 2016, from www.eurolab.org
Guimarães, A.T.B., Silva de Assis, H.C. & Boeger, W. (2007). The effect of trichlorfon on acetycholinesterase activity and his- topathology of cultivated fish Oreochromis niloticus. Ecotoxicology and Environmental Safety, 68, 57-62.
Harnpicharnchai, K., Chaiear, N. & Charerntanyarak, L. (2013). Residues of organophosphate pesticides used in vegetable cultivation in ambient air, surface water and soil in Bueng Niam Subdistrict, Khon Kean Thailand. The Southeast Asian Journal of Tropical Medicine and Public Health, 44, 1088-1097.
Khay, S., Abd El-Aty, A.M., Choi, J.H., Shin, E.H., Shin, C.H., Chang, B.J., Lee, C.H., Shin, S.C., Jeong, J.Y. & Shim, J.H. (2009). Simultaneous determination of pyrethroids from pesticide residues in porcine muscle and pasteurized using GC. Journal of Separation Science, 32, 244-251.
Lehotay, S.J., Lightfield, A.R., Harman-Fetcho, J.A. & Donoghue, D.J. (2001). Analysis of pesticide residues in eggs by direct sample introduction/gas chromatography/tandem mass spectrometry. Journal of Agricultural and Food Chemistry, 49, 4589-4596.
Lertruengdej, Y. & Chongmevasna, P. (1997). Analysis of Trichlorfon in Dry Salted Fish. Bulletin of the Department of Medical Sciences, 39(1), 45-51. (in Thai)
Malone, E.M., Elliott, C.T., Kennedy, D.G.& Regan, L. (2010). Rapid confirmatory method for the determination of sixteen synthetic growth promoters and bisphenol A in bovine milk using dispersive solid-phase extraction and liquid chromatographytandem mass spectrometry. Journal of Chromatography B, 878, 1077- 1084.
Ngoh, M.A. & Cullison, R. (1996). Determination of trichlorfon and dichlorvos residues in shrimp using gas chromatography with nitrogen-phosphorus detection. Journal of Agricultural and Food Chemistry, 44, 2686-2689.
Nordtest, R. (2004). Handbook for Calculation of Measurement Uncertainty in Environmental Laboratories. Retried January 15, 2016, from http://www.nordicinnovation.net/nordtestfiler/tec537.pdf
Park, J.W., Abd El-Aty, A.M., Lee, M.H., Song, S.O. & Shim, J.H. (2006). Residue Analysis of organophosphorus and organochlorine pesticides in fatty matrices by gas chromatography coupled with electron-capture detection. Zeitschrift für Naturforschung, 61c: 341D346.
Pico, Y., Font, G., Molto, J.C. & Manes, J. (2000). Pesticide residue determination in fruit and vegetables by liquid chromatography-mass spectrometry. Journal of Chromatography A, 16, 153D173.
SANCO. (2012). European Commission Health & Consumer Protection Directorate-Gener. Safety of the food chain Chemicals, contaminants, pesticides. Retried January 15, 2016, from http://ec.europa.eu/food/plant/pesticides/guidance_documents/docs/qualcontrol_en.pdf
Sultatos, L.G. (1994). Mammalian toxicology of organophosphorus pesticides. Journal of Toxicology and Environmental Health, Part A, 43, 271D289.
Thoophom, G., Sungvaranond, B., Atisook K., Lertruengdej, Y., Kaewklapanyachareon, L., Suntudrob, J., Chongmevasna, P. & Boonthai, R. (1995). Pesticide and PCB Residues in Foods, 1991-1993. Bulletin of the Department of Medical Sciences, 37(2), 145-160. (in Thai)
Zrostlíkovµ, J., Lehotay, S.J.& HajsÏlovµ, J. (2002). Simultaneous analysis of organophosphorus and organochlorine pesticides in animal fat by gas chromatography with pulsed flame photometric and micro-electron capture detectors. Journal of Separation Science, 25, 527-537.
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2016-06-29
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