Journal of Applied Biological Chemistry

The Korean Society for Applied Biological Chemistry (한국응용생명화학회)
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Development of LC-MS/MS analytical methods for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai

LC-MS/MS를 이용한 생약 백출 및 우슬 중 Metalaxyl 잔류분석법 개발

  • Yun, Myung-Sub (Department of Bio-Environmental Chemistry, College of Agriculture and Food Sciences, Wonkwang University) ;
  • Yang, Seung-Hyun (Department of Bio-Environmental Chemistry, College of Agriculture and Food Sciences, Wonkwang University) ;
  • Choi, Hoon (Department of Bio-Environmental Chemistry, College of Agriculture and Food Sciences, Wonkwang University)
  • Received : 2021.11.18
  • Accepted : 2022.01.17
  • Published : 2022.03.31
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Abstract

A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH2) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r2) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

생약 중 잔류농약의 안전성을 확보하기 위해 metalaxyl에 대해 백출과 우슬의 잔류농약 분석법을 개발하고자 하였다. LC-MS/MS를 사용하여 QuEChERS법을 기반으로 백출과 우슬 중 metalaxyl을 분석하기 위하여 물로 습윤화 시켜 acetonitirile로 추출하여 MgSO4와 NaCl을 첨가해 층 분리 후 SPE-NH2 cartridge로 정제하였다. 본 분석법의 기기정량한계와 분석정량 한계는 0.002 ㎍/mL과 0.01 mg/kg이었고 표준검량선은 0.001-0.05 mg/L 범위에서 결정계수(R2) 0.999의 직선성을 확인하였다. 백출과 우슬에 대한 회수율은 MLOQ 수준, MLOQ의 10배 수준에서 88.1-109.1%의 우수한 회수율을 보였고, 변이계수는 2.0-6.2%로 10%이하였다. 본 연구에서 확립한 LC-MS/MS를 이용한 잔류분석법의 회수율 및 분석오차는 국제적인 기준을 만족하고 있으므로 생약 백출 및 우슬 중 metalaxyl의 안전성 검사를 위한 분석법으로 활용할 수 있을 것이라고 판단된다.

Keywords

Acknowledgement

본 연구는 2020년도 식품의약품안전처의 연구개발비(19172한생약196)로 수행되었으며 이에 감사를 표합니다.

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