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축산물 중 Thiodicarb와 대사산물 Methomyl의 동시분석법개발

Development of Simultaneous Analytical Method for Thiodicarb and its Metabolite Methomyl in Livestock Products

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주제분류농학

초록

BACKGROUND: Agricultural use and pest control purposes of pesticides may lead to livestock products contamination. Thiodicarb and its degraded product, methomyl, are carbamate insecticides that protect soya bean, maize, fruit, and vegetables and control flies in animal and poultry farms. For maximum residue limit enforcement and monitoring, the JMPR residue definition of thiodicarb in animal products is the sum of thiodicarb and methomyl, expressed as methomyl. This residue definition was set to consider the fact that thiodicarb was readily degraded to methomyl in animal commodities. And therefore the simultaneous analytical method of thiodicarb and methomyl is required for monitoring in livestock products. METHODS AND RESULTS: The study was conducted using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and HPLC-MS/MS to determine the thiodicarb and methomyl in livestock products. The limit of quantitation (LOQ) was 0.01 mg/kg for livestock products, including beef, pork, chicken, milk, and egg. The coefficient of determinations (r2) for the calibration curve were > 0.99, which was acceptable values for linearity. Average recoveries at spiked levels (LOQ, 10LOQ, and 50LOQ, n=5) in triplicate ranged from 73.2% to 102.1% and relative standard deviations (RSDs) were less than 10% in all matrices. CONCLUSION: The analytical method was validated for the performance parameters (specificity, linearity, accuracy, and precision) in livestock products to be acceptable by the CODEX guidelines.

Abstract

BACKGROUND: Agricultural use and pest control purposes of pesticides may lead to livestock products contamination. Thiodicarb and its degraded product, methomyl, are carbamate insecticides that protect soya bean, maize, fruit, and vegetables and control flies in animal and poultry farms. For maximum residue limit enforcement and monitoring, the JMPR residue definition of thiodicarb in animal products is the sum of thiodicarb and methomyl, expressed as methomyl. This residue definition was set to consider the fact that thiodicarb was readily degraded to methomyl in animal commodities. And therefore the simultaneous analytical method of thiodicarb and methomyl is required for monitoring in livestock products. METHODS AND RESULTS: The study was conducted using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and HPLC-MS/MS to determine the thiodicarb and methomyl in livestock products. The limit of quantitation (LOQ) was 0.01 mg/kg for livestock products, including beef, pork, chicken, milk, and egg. The coefficient of determinations (r2) for the calibration curve were > 0.99, which was acceptable values for linearity. Average recoveries at spiked levels (LOQ, 10LOQ, and 50LOQ, n=5) in triplicate ranged from 73.2% to 102.1% and relative standard deviations (RSDs) were less than 10% in all matrices. CONCLUSION: The analytical method was validated for the performance parameters (specificity, linearity, accuracy, and precision) in livestock products to be acceptable by the CODEX guidelines.

참고문헌 (11)

  1. 한성수, "살충제 thiodicarb의 단감 중 잔류분석 및 안전성 평가", 농약과학회지, 8(3), pp.184~188 (2004), 한국농약과학회
  2. 최원조, "GC-MS", MS를 이용한 축산물 중 29종 농약의 동시다성분 분석법 검증, 2020, pp.24(2), 196~217[DOI]
  3. 이한솔, "QuEChERS법과 LC-MS", MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증, 2019, pp.34(2), 115~123[DOI]
  4. 서은경, "QuEChERS 전처리와 LC-MS", MS를 이용한 고추 중 침투성농약Imidacloprid 및 대사물질 동시분석법, 2013, pp.17(4), 264~270[DOI]
  5. 김양현, "QuEChERS 시료 처리법을 활용한 엽채류 중 잔류농약분석", 농약과학회지, 16(2), pp.121~130 (2012), 한국농약과학회[DOI]
  6. Tomlin C. D. S, "The Pesticide Manual, eighteenth edition" (2018), British Crop ProductionCouncil (BCPC)
  7. Report of the 2001Joint Meeting of the FAO Panel of Experts on Pesticide Residues in Food and the Environment and the WHO Core Assessment Group, "Pesticide Residues in food", FAO, 163~ (2001)
  8. 박지수, "수박 중 Pyridalyl 및 Fluopicolide의 잔류 특성 및 생물학적 반감기 산출", 한국환경농학회지, 36(1), pp.50~56 (2017), 한국환경농학회[DOI]
  9. Wu Y, "Simultaneous determination of thiodicarb and its main metabolite residues in cotton by ultra-performance liquid chromatography coupled to tandem mass spectrometry", Analytical Methods, 5, pp.1052~1057 (2013)[DOI]
  10. 권혜영, "QuEChERS 전처리법과 HPLC-MS", MS 기기분석을 이용한 사과와 상추 중 240종 농약의 동시분석, 2011, pp.15(4), 417~433[DOI]
  11. Lee SM, "Changes of egg quality during storage", Korean Journal of Veterinary Service, 25(1), pp.15~22 (2002)

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