建立同时测定花生油中4种黄曲霉毒素(包括黄曲霉毒素B1、B2、G1、G2)的液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC.MS/MS)。该方法经甲醇一水、三氯甲烷依次提取样品,以C18柱分离,流动相为乙腈-0.1%甲酸溶液(梯度洗脱),采用电喷雾正离子多反应监测(multiple reactionmonitor,MRM)模式检测。结果表明:标准曲线在0.0~20.0μg/kg进样范围内线性良好;用本法测定4种黄曲霉毒素的回收率在70.8%-108.0%(低加标水甲)、82,4%4104.5%(中和高加标水甲)之间,相对标准偏差在5.7%~9.7%之间。运用所建立的方法对市售19种不同品牌和批次的花生油中的黄曲霉毒素进行分析,结果显示该方法选择性强、灵敏度高,适用于花生油中4种黄曲霉毒素的定性、定量测定。
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for simultaneous determination of 4 aflatoxins in peanut oil including aflatoxins B1, B2, G1 and G2. The sample preparation was achieved by sequential extraction with aqueous methanol solution and chloroform. The analytes were separated on a C18 column using a mobile phase composed of acetonitrile and 0.1% aqueous formic acid solution and detected using electrospray ionisation (ESI)- MS/MS in positive ion mode with multiple reaction monitoring (MRM). The linear range of aflatoxins determination was from 0.0 to 20.0 μ g/kg. The recovery rates for four aflatoxins were from 70.8% to 108.0% at 1,0μg/kg and from 82.4% to 104.5% at 10.0 and 20.0 μ g/kg, and the relative standard deviations from 5.7% to 9.7%. The developed method proved highly selective and sensitive in determining 19 commercial peanut oil samples, thus being suitable for qualitative and quantitative analysis of four aflatoxins in peanut oil.