LC-MS/MS를 이용한 식품 중 맥각 알칼로이드 시험법 개발

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.