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Development of Analytical methods for Chinomethionat in Livestock Products

축산물 중 살균제 Chinomethionat의 개별 잔류분석법 확립

  • Yang, Seung-Hyun (Department of Bio-Environmental Chemistry, College of Agriculture and Food Sciences, Wonkwang University) ;
  • Kim, Jeong-Han (Department of Agricultural Biotechnology and Research Institute of Agriculture and Life Sciences, Seoul National University) ;
  • Choi, Hoon (Department of Bio-Environmental Chemistry, College of Agriculture and Food Sciences, Wonkwang University)
  • 양승현 (원광대학교 농식품융합대학 생물환경화학과) ;
  • 김정한 (서울대학교 농업생명과학대학 농생명공학부) ;
  • 최훈 (원광대학교 농식품융합대학 생물환경화학과)
  • Received : 2021.06.04
  • Accepted : 2021.06.23
  • Published : 2021.06.30

Abstract

BACKGROUND: The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION: The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r2>0.995) in the range of 0.01-0.2 ㎍/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.

본 연구는 축산물 중 퀴녹사린계 살균제 chinomethionat의 잔류분석법을 확립하였다. 소고기, 돼지고기, 닭고기, 우유, 계란을 대표 시료로 선정하고 GC-ECD를 이용한 chinomethionat 단성분 정량 시험법을 개발하였다. 축산물 중 chinomethionat 잔류물을 acetone/dichloromethane (9/1, v/v)로 추출하고 추출첨가제 MgSO4 및 NaCl을 첨가한 후, dichloromethane로 분배하고 Florisil 흡착제로 정제하였다. 축산물 중 chinomethionat 정량한계는 0.02 mg/kg으로 결정되었으며, MLOQ 수준의 회수율은 84.8-100.9%, MLOQ 10배 수준에서는 85.7-103.0%의 우수한 회수율을 보였으며, 분석오차는 최대 5.2%로 재현성 역시 양호하였다. 본 연구에서 확립한 chinomethionat의 잔류분석법은 국내·외 축산물의 잔류농약 검사 및 분석에 적용 가능할 것으로 기대된다.

Keywords

Acknowledgement

This research was supported by the Ministry of Food and Drug Safety, Republic of Korea (grant number: 16162MFDS586).

References

  1. Vettorazzi, G. (1977). State of the art of the toxicological evaluation carried out by the joint FAO/WHO expert committee on pesticide residues. III. Miscellaneous pesticides used in agriculture and public health. Residue Reviews, 137-184. https://doi.org/10.1007/978-1-4612-6352-4_4.
  2. Tseng S, Lin Y, Lee H, Su S, Chou S, Hwang D (2007) A multiresidue method for determining 136 pesticides and metabolites in fruits and vegetables: Application of macroporous diatomaceous earth column. Journal of Food and Drug Analysis, 15(3), 316-324.
  3. Okihashi M, Kitagawa Y, Akutsu K, Obana H, Tanaka Y (2005) Rapid method for the determination of 180 pesticide residues in foods by gas chromatography/mass spectrometry and flame photometric detection. Journal of Pesticide Science, 30(4), 368-377. https://doi.org/10.1584/jpestics.30.368.
  4. Park JW, Kim AK, Kim JP, Lee HH, Park DW, Moon SJ, Ha DR, Kim ES, Seo KW (2014) Multi-residue analysis of pesticides using GC-TOF/MS, ECD, NPD with QuECHERS sample preparation. The Korean Journal of Pesticide Science, 18(4), 278-295. https://doi.org/10.7585/kjps.2014.18.4.278.
  5. Vargas-Perez M, Dominguez I, Gonzalez FJE, Frenich AG (2020) Application of full scan gas chromatography high resolution mass spectrometry data to quantify targeted-pesticide residues and to screen for additional substances of concern in fresh-food commodities. Journal of Chromatography A, 1622, 461118. https://doi.org/10.1016/j.chroma.2020.461118.
  6. Kim YJ, Choi YH, Shin BW, Lee JH (2011) Comparison between the liquid-liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat. Korean Journal of Veterinary Service, 34(4), 429-439. https://doi.org/10.7853/kjvs.2011.34.4.429.
  7. Wu CC (2017). Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry. Food Chemistry, 229, 580-587. https://doi.org/10.1016/j.foodchem.2017.02.081.
  8. Hildmann F, Gottert C, Frenzel T, Kempe G, Speer K (2015) Pesticide residues in chicken eggs-A sample preparation methodology for analysis by gas and liquid chromatography/tandem mass spectrometry. Journal of Chromatography A, 1403, 1-20. https://doi.org/10.1016/j.chroma.2015.05.024.
  9. Sturm J, Wienhold P, Frenzel T, Speer K (2018) Ultra turrax ® tube drive for the extraction of pesticides from egg and milk samples. Analytical and Bioanalytical Chemistry, 410, 5431-5438. https://doi.org/10.1007/s00216-018-1254-9.
  10. Chuang WC, Chen JW, Huang CH, Shyu TH, Lin SK (2019) FaPEx ® Multipesticide residues extraction kit for minimizing sample preparation time in agricultural produce. Journal of AOAC International, 102(6), 1864-1876. https://doi.org/10.1093/jaoac/102.6.1864.
  11. Nutahara M, Murai T (1984) Accelerating effect of natural unsaturated fatty acids on photodecomposition of chinomethionat (Morestan ®). Journal of Pesticide Science, 9(4), 667-674. https://doi.org/10.1584/jpestics.9.667.
  12. Mastovska K, Lehotay SJ (2004) Evaluation of common organic solvents for gas chromatographic analysis and stability of multiclass pesticide residues. Journal of Chromatography A, 1040(2), 259-272. https://doi.org/10.1016/j.chroma.2004.04.017.
  13. Katagi T (2004) Photodegradation of pesticides on plant and soil surfaces. Reviews of Environmental Contamination and Toxicology, 1-78. https://doi.org/10.1007/978-1-4419-9098-3_1.