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http://dx.doi.org/10.12719/KSIA.2018.30.4.339

Development of Individual Residue Analysis Method for Cyanazine in Agricultural Commodities as an Unregistered Herbicide in Korea  

Choung, Myoung-Gun (Department of Herbal Medicine Resource, Kangwon National University)
Im, Moo-Hyeog (Department of Food Engineering, Daegu University)
Publication Information
Journal of the Korean Society of International Agriculture / v.30, no.4, 2018 , pp. 339-346 More about this Journal
Abstract
Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.
Keywords
Cyanazine; HPLC-DAD/MS; Residue;
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1 Lynch, S.M., Rusiecki, J.A., Blair, A., Dosemeci, M., Lubin, J., Sandler, D., Hoppin, J.A., Lynch, C.F., & Alavanja, M.C. 2006. Cancer incidence among pesticide applicators exposed to cyanazine in the agricultural health study. Environmental Health Perspectives 114(8): 1248-1252.   DOI
2 McLafferty, F.W., & Turecek, F. 1993. Interpretation of mass spectra, pp. 19-50, 4th ed. Sausalito, CA, USA.
3 Meador, M., & Jie, M. 2014. Maximum residue limits for pesticides in food, p. 130, Beijing, China.
4 NewZealand Food Safety Authority. 2007. Technical information sheets for purposed MRLs, p. 8.
5 Ministry of Food and Drug Safety. 2017. Korea Food Code, pp. 10-4-340-10-4-342.
6 Park, H.K., Noh, H.H., Lee, K.H., Lee, J.Y., Park, Y.S., Kang, K.W., Lee, E.Y., Yun, S.S., Jin, C.W., & Kyung, K.S. 2011. Residual characteristic of chlorpyrifos in squash and estimation of its residues before harvest, Korean Journal of Pesticide Science 15(4): 463-470.
7 Sanchez-Rasero, F., & Dios, G.C. 1988. Liquid chromatographic method for the determination of cyanazine in the presence of some normal soil constituents, Journal of Chromatography 447: 426-431.   DOI
8 US FDA. 1999. Pesticide Analytical Manual, Vol 1: Multi-residue Methods (3rd ed.), US Food and Drug Administration, USA.
9 World Health Organization. 2003. Cyanazine in drinking-water, Background document for development of WHO guidelines for drinking-water quality, p. 1, 2nd ed. Geneva, Switzerland.
10 Zhang, G., & Pan, J. 2011. Simultaneous spectrophotometric determination of atrazine and cyanazine by chemometric methods, Spectrochimica Acta Part A. 78, 238-242.   DOI
11 Hwang, Y.S., Lim, J.D., & Choung, M.G. 2016. Analytical method for triazine herbicide cyanazine residues in major medicinal crops. Korean Journal of Medicinal Crop Science 14(3): 237-245.
12 AOAC. 2000. Pesticide and industrial chemical residues, In Official method of analysis, pp. 1-88. 17th ed., AOAC International, Arlington, VA, USA.
13 Codex Alimentarius Commission. 2003. Guidelines on Good Laboratory Practice in Residue Analysis, CAC/GL 40-1993, Rev.1-2003, Rome, Italy.
14 Hogendoorn, E.A., & Goewie, C.E. 1989. Residue analysis of the herbicides cyanazine and bentazone in sugar maize and surface water using high-performance liquid chromatography and an online clean-up column-switching procedure. Journal of Chromatography 475: 432-441.   DOI
15 Lee, S.J., Kim, Y.H., Song, L.S., & Choung, M.G. 2011 a. Determination of ametryn residue in agricultural commodities using HPLC-UVD/MS, Korean Journal of Pesticide Science 15(2): 125-133.
16 Kwon, C.H., Chang, M.I., Im, M.H., Choi, H., Jung, D.I., Lee, S.C., Yu, J.Y., Lee, Y.D., Lee, J.O., & Hong, M.K. 2008. Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry. Analytical Science & Technology 21(6): 518-525.
17 Lee, J.H., Park, H.W., Keum, Y.S., Kwon, C.H., Lee, Y.D., & Kim, J.H. 2008. Dissipation pattern of boscalid in cucumber under greenhouse condition. Korean Journal of Pesticide Science 12(1): 67-73.
18 Lee, S.J., Hwang, Y.S., Kim, Y.H., Nam, M.Y., Hong, S.B., Yun, W.K., Kwon, C.H., Do, J.A., Im, M.H., Lee, Y.D., & Choung, M.G. 2010. Determination of formesafen residue in agricultural commodities using HPLC-UVD/MS, Korean Journal of Pesticide Science 14(2): 100-108.
19 Lee, Y.D. 2017. Pesticide Analytical Residues Manual in Food Code. Ministry of Food and Drug Safety, Seoul, Korea.
20 Lee, S.J., Kim, Y.H., Song, L.S., Hwang, Y.S., Lim, J.D., Sohn, E.H., Im, M.H., Do, J.A., Oh, J.H., Kwon, K.S., Lee, J.K., Lee, Y.D., & Choung, M.G. 2011 b. Development of analytical method for fenoxycarb, pyriproxyfen and methoprene residues in agricultural commodities using HPLC-UVD/MS. Korean Journal of Pesticide Science 15(3): 254-268.