Browse > Article
http://dx.doi.org/10.5338/KJEA.2012.31.2.157

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-  

Chang, Hee-Ra (Environmental Chemistry, HTRC, Hoseo Universitiy)
Kang, Hae-Rim (Environmental Chemistry, HTRC, Hoseo Universitiy)
Kim, Jong-Hwan (Environmental Toxicology Center, Korea Institute of Toxicology, KRICT)
Do, Jung-A (National Institute of Food and Drug Evaluation)
Oh, Jae-Ho (National Institute of Food and Drug Evaluation)
Kwon, Ki-Sung (National Institute of Food and Drug Evaluation)
Im, Moo-Hyeog (Korea Food and Drug Administration)
Kim, Kyun (Environmental Chemistry, HTRC, Hoseo Universitiy)
Publication Information
Korean Journal of Environmental Agriculture / v.31, no.2, 2012 , pp. 157-163 More about this Journal
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 $R^2$ >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 0.5 mg/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 0.5 mg/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.
Keywords
Brown rice; GC-ECD; Mass Spectrometry; Multiresidue; Orange; Pesticide;
Citations & Related Records
연도 인용수 순위
  • Reference
1 Pang G.-F., Fan C.-L., Liu Y.-M., Cao Y.-Z., Zhang J.-J., Fu B.-L., Li X.-M., Li Z.-Y., Wu Y.-P., 2006. 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, Food Additives and Contaminants 23(8), 777-810.   DOI   ScienceOn
2 Polese L., Ribeiro M.L., 1998. Methods for determination of hexachlorobenzene and penta-chlorophenol in soil samples, Talanta 46, 915-920.   DOI   ScienceOn
3 Syngenta, 2006. Determination of hexachlorobenzene and decachlorobiphenyl in technical and formulated chlorothalonil, Adapted from document 4377m, presented by Syngenta to the CIPAC meeting in Brno, June 2004.
4 The Japan Food Chemical Research Foundation, Positive List System for Agricultural Chemical Residues in Food (http://m5.ws001.squarestart.ne.jp/zaidan/search.html)
5 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.
6 Tomlin, C.D.S, 2009. The Pesticide Manual (15th), pp208-209, 222-223, 362-363, 610-611, 908-909, 960-961.
7 Xu X.-L, Li L., Zhong W.-K., He Y.-J., 2009. Multiresidue analysis of 205 crop pesticides using minisolid phase extraction-large volume injection- GC-MS, Chromatographia 70(1/2), 173-183.   DOI
8 Pesticide Residue Analytical Methods Research Committee, 2006. The Newest Pesticide Residue Analytical Methods, revised version.
9 Korea Food and Drug Administration (KFDA), 2010. Analytical methods of pesticide residues in foods.
10 Codex Alimentarius, 2010. FAO/WHO Food Standard (http://www.codexalimentarius.net/pestres/data/index.html?lang=en)
11 European Commission, 2009. DG Sanco 2008 European Commission Regulation(EC) No. 1107/2009 (http://ec.europa.eu/sanco_pesticides/public/index.cfm?event=substance.selection)
12 Fenoll J., Hellin O., Lopez J., Gonzales A., and Flores P., 2007. Determination of pesticide residues in lettuce by gas chromatography with electron-capture detection, J. AOAC Int. 90(6), 1670-1676.
13 Hirahara Y., Kimura M., Inoue T., Uchikawa S., Otani S., Haganuma A., Matsumoto N., Hirata A., Maruyama S., Iizuka T., Ukyo M., Ota M., Hirose H., Suzuki S., and Uchida Y., 2005. Validation of multiresidue screening methods for the determination of 186 pesticides in 11 agricultural products
14 Japan Ministry of Health, Labour and Welfare Department of Food Safety, 2006. 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.).
15 Caballo-Lopez A., Luque de Castro M.D., 2006. 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, 341-345.   DOI
16 Kawata K., Asada T., Tanabe A., Oikawa K., 2005. Runoff of clomeprop and oxaziclomefone from a paddy field, Bull. Environ. Contam. Toxicol. 75, 922-928.   DOI
17 Kobayashi K., Tsukasaki Y., Tongma S., and Shim I.S., 1999. Phytotoxic activity of clomeprop in soil and concentration of its hydrolysed metabolite DMPA in soil water, Pesticide Science 55, 474-478.   DOI
18 Murano H., Kobayashi K., and Fujihara S., 2007. Residual activity of clomeprop and its downward movement under laboratory conditions, Weed Biology and Management 7, 201-208.   DOI   ScienceOn
19 Alder L., Greulich K., Kempe G., and Vieth B., 2006. Residue analysis of 500 high priority pesticides: Better by GC-MS or LC-MS/MS?, Mass Spectrometry Reviews 25, 838-865.   DOI   ScienceOn