CAJ | 학술논문

目的：建立饼干中4种单端孢霉烯类真菌毒素的液相色谱-质谱联用分析方法。方法样品经乙腈/水溶液(84：16, V：V)提取后用MycoSep?227或 MycoSep?226多功能柱净化, Agilent ZORBAX Bonus-RP色谱柱分离,液相色谱-质谱联用(LC-MS/MS)测定,电喷雾正离子模式(ESI+)和负离子模式(ESI－)多反应模式检测。结果样品中4种单端孢霉烯类真菌毒素在各自的线性范围内线性关系良好,相关系数均不低于0.997,定量限为5~20μg/kg,3个加标水平下平均回收率为66.9%~101.8%,相对标准偏差为3.7%~13.9%。结论该方法具有前处理简单、净化效果好、灵敏度高,适用于同时检测一种样品中4种单端孢霉烯类真菌毒素的残留量。
목적：건립병간중4충단단포매희류진균독소적액상색보-질보련용분석방법。방법양품경을정/수용액(84：16, V：V)제취후용MycoSep?227혹 MycoSep?226다공능주정화, Agilent ZORBAX Bonus-RP색보주분리,액상색보-질보련용(LC-MS/MS)측정,전분무정리자모식(ESI+)화부리자모식(ESI－)다반응모식검측。결과양품중4충단단포매희류진균독소재각자적선성범위내선성관계량호,상관계수균불저우0.997,정량한위5~20μg/kg,3개가표수평하평균회수솔위66.9%~101.8%,상대표준편차위3.7%~13.9%。결론해방법구유전처리간단、정화효과호、령민도고,괄용우동시검측일충양품중4충단단포매희류진균독소적잔류량。
ABSTRACT:Objective To establish a simultaneous determination method for 4 kinds of trichothecenes in cookies by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were sequentially extracted by 84% acetonitrile-water solution(V:V), cleaned up with MycoSep?227 or MycoSep?226, and separated by Agilent ZORBAX Bonus-RP column and detected by LC-MS/MS. The MS conditions used were negative (ESI+) and positive (ESI-) electrospray ionization and MRM models. Results This method showed a good linearity within their respective linear ranges with high correlation coefficients (r2≥0.997) of 4 trichothecenes, and the detection limits for them were ranged from 5 to 20 μg/kg, the average recoveries in the above 3 matrices spike at 3 levels were between 66.9% to 101.8%, with a relative standard deviation (RSD) were in the range from 3.7% to 13.9%. Conclusion This analytical method can meets the requirements for trace assays. In addition, it is simple, rapid, accurate and suitable for the simultaneous determination of 4 kinds of trichothecenes in cookies.