粮谷中8种痕量真菌毒素的定量分析方法

Accurate Quantitative Analysis Method for 8 Kinds of Mycotoxins in Cereal

建立了大米、小麦和大豆中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、伏马毒素B1、伏马毒素B2、柄曲霉素和异烟棒曲霉素C 8种真菌毒素的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品加入正己烷去除油脂,用60%乙腈振荡液液分配提取,取乙腈水层过滤膜后分析。在电喷雾电离(ESI)正离子模式下采用多反应监测(MRM)进行测定。定量方法采用同位素内标稀释法,8种真菌毒素在各自浓度范围内线性关系良好,线性系数均不低于0.997 0。空白样品的加标回收率为77%～123%,相对标准偏差(RSD)为0.6%～13.3%。该方法操作简单、灵敏度高,可用于粮谷中真菌毒素的检测。

A high performance liquid chromatography- tandem mass spectrometric （HPLC -MS/MS） method was developed for the determination of 8 kinds of mycotoxins（ aflatoxin B1, aflatoxin B2, af- latoxin G1, aflatoxin G2, fumonisin B1, fumonisin B2, real. The sample was diluted with hexane to remove the The acetonitrile layer was made up to constant volume and sterigmatocystin and roquefortine C） in ce- oil, then extracted with 60% acetonitrile. passed through the filter before tested. The detection was performed in the electrospray ion positive mode and multiple reaction monitoring（MRM） mode, and the quantitation of target compounds was carried out by the isotope dilution assays. The results indicated that the 8 compounds showed good linear relationships in certain concentration ran- ges, with correlation coefficients not less than than 0. 997 O. The average recoveries ranged from 77% to 123% , with relative standard deviations of 0. 6% - 13.3%. The method was proved to be rapid and sensitive, and could be used for the detection of mycotoxins in cereal.