Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Development of Analytical Method for Ergot Alkaloids in Foods Using Liquid Chromatoraphy-Tandem Mass Spectrometry

LC-MS/MS를 이용한 식품 중 맥각 알칼로이드 시험법 개발

  • Chun, So Young (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chong, Euna (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Bomnae (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kwon, Jin-Wook (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Park, Hye Young (Herbal Medicine Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food Drug Safety) ;
  • Kim, Sheenhee (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Gang, Giljin (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 천소영 (식품의약품안전처 식품의약품안전평가원 오염물질과) ;
  • 정은아 (식품의약품안전처 식품의약품안전평가원 오염물질과) ;
  • 이봄내 (식품의약품안전처 식품의약품안전평가원 오염물질과) ;
  • 권진욱 (식품의약품안전처 식품의약품안전평가원 오염물질과) ;
  • 박혜영 (식품의약품안전처 식품의약품안전평가원 생약연구과) ;
  • 김신희 (식품의약품안전처 식품의약품안전평가원 오염물질과) ;
  • 강길진 (식품의약품안전처 식품의약품안전평가원 오염물질과)
  • Received : 2019.02.26
  • Accepted : 2019.04.05
  • Published : 2019.04.30
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Abstract

Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.

우리나라의 해외 곡류 수입량과 수입국가의 다변화를 고려 해 볼 때, 호밀, 밀, 귀리 등 맥류에서 주로 발생하는 것으로 알려져 있는 맥각알칼로이드의 노출가능성도 배제할 수 없다. 따라서 본 연구는 곡류 및 곡류가공품 중 맥각알칼로이드에 대한 선제적 안전관리를 위해 호밀 및 가공품 (크래커, 맥주) 으로 부터 에르고메트린을 포함한 12종 맥각알칼로이드의 공인 시험법을 개발하고자 하였다. 아세토니트릴이 함유된 2 mM 탄산암모늄용액 추출과 Mycocep catridge를 이용한 정제 농축이 전처리 방법으로 적합함이 확인되었고, 기기분석을 통해 표준물질 첨가 검량선의 직선성이 12개 알칼로이드 모두 $R^2$ >0.99 이상이었으며, 정량한계는 $0.01{\sim}0.05{\mu}g/kg$수준이었다. 시험법 검증을 통해 대상 품목간의 차이는 있으나, 12개 맥각 알칼로이드 모두 회수율은 72~113% 수준이었으며, 반복성은 2~10% 수준으로 적합성이 확인되었다.

Keywords

References

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