우리나라의 해외 곡류 수입량과 수입국가의 다변화를 고려 해 볼 때, 호밀, 밀, 귀리 등 맥류에서 주로 발생하는 것으로 알려져 있는 맥각알칼로이드의 노출가능성도 배제 할 수 없다. 따라서 본 연구는 곡류 및 곡류가공품 중 맥 각알칼로이드에 대한 선제적 안전관리를 위해 호밀 및 가공품 (크래커, 맥주) 으로 부터 에르고메트린을 포함한 12 종 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 R2 >0.99 이상이 었으며, 정량한계는 0.01 ~ 0.05 μg/kg수준이었다. 시험법 검증을 통해 대상 품목간의 차이는 있으나, 12개 맥각 알칼로이드 모두 회수율은 72~113% 수준이었으며, 반복성은 2~10% 수준으로 적합성이 확인되었다.

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; R2 >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and 100 μg/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 μg/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.

ABSTRACT
 Materials and Methods
  시약 및 재료
  표준원액 및 표준용액의 조제
  시료 전처리 방법
  기기분석조건
  시험법 검증
 Results and Discussion
  LC-MS/MS 분석조건 최적화
  추출 및 정제조건 확립
  분석법 검증
 국문요약
 References

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