식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-
Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-
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초록
BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl,clomeprop, diflufenican, hexachlorobenzene, picolinafen,and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02∼0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were R2 >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2∼8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2∼6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.
Abstract
BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl,clomeprop, diflufenican, hexachlorobenzene, picolinafen,and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02∼0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were R2 >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2∼8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2∼6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.
참고문헌 (19)
- Alder L., "Residue analysis of 500 high priority pesticides: Better by GC-MS or LC-MS", MS, 2006, pp.25, 838~865
- Caballo-Lopez A., "Gas chromatography-electron capture detection determination of Dacthal and its di-acid metabolite in soil after ultrasound-assisted extraction and in situ focused microwave-assisted derivatization", Anal. Bioanal. Chem, 386, pp.341~345 (2006)
- "FAO/WHO Food Standard"[URL]
- "DG Sanco 2008 European Commission Regulation(EC) No. 1107"[URL]
- Fenoll J., "Determination of pesticide residues in lettuce by gas chromatography with electron-capture detection", J. AOAC Int, 90(6), pp.1670~1676 (2007)
- Hirahara Y., "Validation of multiresidue screening methods for the determination of 186 pesticides in 11 agricultural products", ~ (2005)
- Japan Ministry of Health, Labour and Welfare Department of Food Safety, "Analytical Methods for Residual Compositional Substances of Agricultural Chemicals", Feed Additives, and Veterinary Drugs in Food(Syoku-An No.0124001, January 24, 2005. Final amendments were made on May 26, 2006.), ~ (2006)
- Kawata K., "Runoff of clomeprop and oxaziclomefone from a paddy field", Bull. Environ. Contam. Toxicol, 75, pp.922~928 (2005)
- Kobayashi K., "Phytotoxic activity of clomeprop in soil andconcentration of its hydrolysed metabolite DMPAin soil water", Pesticide Science, 55, pp.474~478 (1999)
- Murano H., "Residual activity of clomeprop and its downward movement under laboratory conditions", Weed Biology and Management, 7, pp.201~208 (2007)
- Pang G.-F., "Multi-residue method for the determination of 450 pesticide residues in honey, fruit juice and wine by double-cartridge solid-phase extraction", gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry, 2006, pp.23(8), 777~810
- Polese L., "Methods for determination of hexachlorobenzene and penta-chlorophenol in soil samples", Talanta, 46, pp.915~920 (1998)
- Syngenta, "Determination of hexachlorobenzene and decachlorobiphenyl in technical and formulated chlorothalonil, Adapted from document 4377m", presented by Syngenta to the CIPAC meeting in Brno (2006)
- "Positive List System for Agricultural Chemical Residues in Food"[URL]
- The Office of the Federal Register, "Nation Archives and Records Administration, 2010", 40 Electronic Code of Federal Regulation Part 150 to 189, 180.1 to 180.2020, ~ (2010)
- Tomlin, C.D.S, "The Pesticide Manual (15th)", 208~209 (2009)
- Xu X.-L, "Multiresidue analysis of 205 crop pesticides using minisolid phase extraction-large volume injection- GC-MS", Chromatographia, 70(1), pp.173~183 (2009)
- Pesticide Residue Analytical Methods Research Committee, "The Newest Pesticide Residue AnalyticalMethods", revised version, ~ (2006)
- Korea Food and Drug Administration (KFDA), "Analytical methods of pesticide residues in foods", ~ (2010)