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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6 min内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B1、黄曲霉毒素M1、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%,精密度RSD为0.36~4.79%。该方法快速、灵敏,适用于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检测与确证。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) was developed for the determination of aflatoxin B1, aflatoxin M1, deoxynivalenol, ochratoxin A and zearalenone in peanut and its products A rapid method for the analysis of mycotoxins. Samples were extracted with methanol-water (55:45, V / V), extracted with a mycotoxin immunoaffinity column and detected using multiple reaction monitoring (MRM) mode in ESI + mode. The target was effectively separated on a C18 column and a sample was analyzed within 6 min with a correlation coefficient (r2, n = 6) of greater than 0.999. The results were stable and sensitive. The linear range of aflatoxin B1, aflatoxin M1 and deoxynivalenol was 0.5 ~ 50.0μg / L with the detection limits of 0.05μg / kg (LOD, S / N = 3), ochratoxin A The linear range of zearalenone was 5.0-100.0μg / L with the detection limit of 0.5μg / kg (LOD, S / N = 3). The recoveries were 86.8% ~ 102.7% and the RSDs were 0.36 ~ 4.79%. The method is rapid and sensitive and is suitable for the detection and confirmation of five mycotoxins of aflatoxin B1, aflatoxin M1, deoxynivalenol, ochratoxin A and zearalenone in peanut and products.