建立了一种测定蜂花粉中黄曲霉毒素(B1、B2、G1、G2)的液相色谱串联质谱方法。样品经V(乙腈)∶V(水)=60∶40提取,通过低温脂肪沉淀,免疫亲和柱净化,之后用甲醇洗脱4种毒素,氮吹后复溶,采用液相色谱-串联质谱(LC-MS/MS)定量分析。方法在3个浓度添加水平的回收率为74.3%~96.5%,精密度低于10.0%。相关系数(r2)均大于0.997。B1、B2、G1、G2的定量限分别为0.05,0.1,0.013,0.025μg/kg。测定30个实际样品,未检出4种毒素。

A simple and sensitive method has been develop for simultaneous determination of aflatoxins( AFB1,AFB2,AFG1,and AFG2) in bee pollen. The sample was extracted with a mixture of acetonitrile / water( 60 ∶ 40,v /v); fat was precipitated in low temperature,followed by immune affinity column cleanup. The aflatoxins were quantified using liquid chromatography coupled with tandem mass spectrometry( LC-MS / MS) with an electrospray ionization( ESI),and a triple quadrupole( Qq Q) analyzer. Recoveries at three levels were in the range of 74. 3% ~ 96. 5%with RSD less than 10. 0%. The correlation coefficients( r2) of the four aflatoxins were higher than 0. 997. The LOQ of B1,B2,G1 and G2 were 0. 05,0. 1,0. 013,0. 025 g / kg,respectively. The method was simple,accurate and sensitive. It was suitable for quantification and confirmation of aflatoxins in bee pollen samples.