摘要
建立了高效液相色谱-串联质谱（HPLC．MS／MS）测定花生及制品中黄曲霉毒素B1、黄曲霉毒素M1、脱氧雪腐镰刀菌烯醇、赭曲霉毒素A、玉米赤霉烯酮五种真菌霉素的快速分析方法。用甲醇．水（55：45，V／V）对样品进行提取，采用真菌毒素免疫亲和柱萃取，在ESI＋模式下采用多反应监测（MRM）模式进行检测。目标物在C18色谱柱上实现了有效分离，在6minffq完成一个样品的分析，相关系数（r2，n=6）大于0．999，检测结果稳定，灵敏。黄曲霉毒素Bl、黄曲霉毒素Ml、脱氧雪腐镰刀菌烯醇线性范围0．5-50．0μg／L，检出限为0．05μg／kg（LOD，S／N=3），赭曲霉毒素A、玉米赤霉烯酮线性范围5．0---100．0μg／L，检出限为0．5μg／kg（LOD，S／N=3），方法回收率为86．8～102．7％，精密魔RsD为0．360．79％。该方法快速、灵敏，适用于花生及制品中黄曲霉毒素Bl、黄曲霉毒素M1、脱氧雪腐镰刀菌烯醇、赭曲霉毒素A、玉米赤霉烯酮五种真菌霉素的检测与确证。
A method based on high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was developed for simultaneous determination of five mycotoxins, namely aflatoxin Bl （AFB1）, aflatoxin M1 （AFMI）, Deoxynivalenol （DON）, Zearalenone （ZEA） and OchratoxinA （OTA）, in peanut and its products. The samples were extracted with methanol-aqueous solution （55：45, V/V）, cleaned up and enriched by mycotoxin affinity column, and then analyzed by HPLC-MS/MS under the multiple reaction monitoring （MRM） mode. All the analytes were successfully detected in positive ion mode within 6 min, and the correlation coefficients （r2, n=6） were more than 0.999. The linear ranges for AFBb AFMI, and DON were between 0.5μg/L to 50.0 μg/L, with detection limit of （LOD, S/N=3） 0.05 μg/kg. While ZEA and OTA were ranging fi＇om 5.0 μg/L to 100.0μg/L, and the detection limit （LOD, S/N=3） was 0.5μg/kg. The spiked recoveries were in the range of 86.8-102.7%, and relative standard deviations （RSD, n=3） were 0.36-4.79%. The method was simple, effective and sensitive, and was suitable for the determination and confLrmation of five mycotoxins in peanuts and products samples.
出处
《现代食品科技》
EI
CAS
北大核心
2014年第1期217-221,164,共6页
Modern Food Science and Technology
