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High Performance Liquid Chromatographic Method for Determination of Metazosulfuron Residue in Representative Crops
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 Title & Authors
High Performance Liquid Chromatographic Method for Determination of Metazosulfuron Residue in Representative Crops
Lee, Hyeri; Kim, Eunhye; Lee, Young Deuk; Kim, Jeong-Han;
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BACKGROUND: This study was performed to develop a single residue analytical method for new herbicide metazosulfuron in crops. METHODS AND RESULTS: Brown rice, apple, mandarin, Kimchi cabbage and soybean were selected as representative crops, and clean-up system, partition solvent and extraction solvent were optimized. Instrumental limit of quantitation (ILOQ), linearity of calibration curve and method limit of quantitation (MLOQ) were determined based on the chromatography and whole procedures. For recovery tests, brown rice, apple, mandarin, Kimchi cabbage and soybean samples were macerated and fortified with metazosulfuron standard solution at three levels (MLOQ, 10 MLOQ and 100 MLOQ). And then those were extracted with acetonitrile, concentrated, and partitioned with ethyl acetate. Then the extracts were concentrated again and cleaned-up through (aminopropyl) SPE cartridge with acetone : dichloromethane (1% acetic acid) (20 : 80, v/v) before concentration and analysis with HPLC. CONCLUSION(S): ILOQ of metazosulfuron was 2 ng (S/N10) and good linearity was achieved between 0.05 and 12.5 mg/Kg of metazosulfuron standard solutions, with coefficients of determination of 0.9999. MLOQ was 0.02 mg/Kg. Good recoveries from 74.1 to 116.9% with coefficients of variation (C.V.) of less than 10% were obtained, regardless of sample type, which satisfies the criteria of Korea Food and Drug Administration (KFDA). Those results were reconfirmed with LC-MS (SIM). The method established in this study is simple, economic and efficient to be applied to most of crops as an official and general method for residue analysis of metazosulfuron.
High performance liquid chromatography;Limit of quantitation;Metazosulfuron;Method limit of quatitation;Recovery;
 Cited by
Ahmed, F.E., 2001. Analyses of pesticides and their metabolites in foods and drinks, Trac-Trends Anal. Chem. 20, 649-661. crossref(new window)

Codex Alimentarius Commission, 2003. Guidelines on good laboratory practice in pesticide residue analysis. CAC/GL 40-1993. Italy.

Fong, W.G., Moye, H.A., Seiber, J.N., Toth, J.P., 1999. Pesticide Residues in Foods: Methods, Technologies, and Regulations. pp. 3-22, 40-42, John Wiley & Sons, Inc., USA.

Gallitzendorfer, R., Timm, T., Koch, D., Kusters, M., Gerhartz, M., 2011. Simultaneous determination of 12 sulfonylurea herbicides in drinking water after SPE by LC-DAD, Chromatographia. 73, 813-816. crossref(new window)

Hollaway, K.L., Kookana, R.S., McQuinn, D.J., Moerkerk, M.R., Noy, D.M., Smal, M.A., 1999. Comparison of sulfonylurea herbicide residue detection in soil by bioassay, enzyme-linked immunosorbent assay and hplc, Weed res. 39, 383-397. crossref(new window)

Ishimitsu, S., Kaihara, A., Yoshii, K., Tsumura, Y., Nakamura, Y., Tonogai, Y., 2002. Simultaneous determination of azimsulfuron, flazasulfuron and halosulfuron-methyl in grains, seeds, vegetables and fruits by HPLC, J. Health Sci. 48, 335-340. crossref(new window)

Kang, S., Chang, N., Zhao, Y., Pan, C., 2011. Development of a method for the simultaneous determination of six sulfonylurea herbicides in wheat, rice, and corn by liquid chromatography-tandem mass spectrometry, J. Agric. Food Chem. 59, 9776-9781. crossref(new window)

Korea Crop Protection Association (KCPA), 2012. Agrochemicals Use Guide Book, p. 847, Samjeong Printing Co., Korea.

Korea Food and Drug Administration (KFDA), 2012. Food Code. Korea.

Kramer, W., Schirmer, U., Jeschke, P., Witschel, M., 2012. Modern crop protection compounds. pp. 50-75, Wiley-VCH Verlag GmbH & Co. KgaA, Germany. (2012).

Lee, H., Kim, E., Moon, J.K., Zhu, Y.Z., Do, J.A., Oh, J.H., Kwon, K., Lee, Y.D., Kim, J.H., 2012. Establishemnt of analytical method for cyazofamid residue in apple, mandarin, Korean cabbage, green pepper, potato and soybean, J. Korean Soc. Appl. Biol. Chem. 55, 241-247.

Lee, I.Y., Kim, C.S., Lee, J., Moon, B.C., Lee, C.G., 2011. Biological characteristics of new paddy field herbicide metazosulfuron granule for paddy weeds, Korean J. Weed Sci. 31, 308-312. crossref(new window)

Lee, Y.D., 2012. Practical Guide for Food Code pesticide residue analysis, pp. 3, 78-82, KFDA, Korea.

Menne, H.J., Janowitz, K. and Berger, B.M., 1999. Comparison of capillary electrophoresis and liquid chromatography for determination of sulfonylurea herbicides in soil, J. AOAC. Int. 82, 1534-1541.

Miller, J.M., 2005. Chromatography: Concepts and contrasts. pp. 285-296, John Wiley & Son, Inc., USA.

Pesticide Residue Analytical Group (PRAG), 2006. New pesticide residue analytical method. pp. 70-72, Rev. ed. PRAG, Japan.

Saha, S., Singh, S.B., Kulshrestha, G., 2003. High performance liquid chromatographic method for residue determination of sulfosulfuron, J. Environ. Sci. Health B. 38, 337-347. crossref(new window)

Stoytcheva, M., 2011. Pesticide-Strategies for Pesticides Analysis, in: Tan, G.H., Chai, M.K., Sample preparation in the analysis of pesticides residue in food by chromatographic techniques, Intech, Croatia, pp. 27-58.

Torres, C.M., Pico, Y., Manes, J., 1996. Determination of pesticide residues in fruit and vegetables, J. Chromatogr. A. 754, 301-331. crossref(new window)

Ware, G.W., Whitacre, D.M., 2004. The pesticide book. pp. 3-13, sixth ed. Meister Media Worldwide, USA.