LC-MS/MS测定猪尿中的黄曲霉毒素M_1

Determination of aflatoxin M_1 in pig urine by LC-MS/MS

建立LC-MS/MS检测猪尿中黄曲霉毒素M1的含量。猪尿样用超纯水稀释定容,充分漩涡振荡后经免疫亲和层析柱净化,甲醇洗脱,微孔滤膜过滤,经液相色谱分离,电喷雾离子源离子化,多反应离子监测(MRM)方式检测。外标法定量。采用0.1%甲酸:乙腈+甲醇溶液(1+1)为流动相,梯度洗脱。0.3mL/min的流速。在0.01μg/kg～0.50μg/kg范围内具有良好的线性关系,最低检测限为0.01μg/kg,回收率在70%～95%之间。此法操作简便、快速、灵敏、准确、样品处理简便易行,适用于测定猪尿中的黄曲霉毒素M1。

An analytical method for the determination of aflatoxin M1 content in pig urine by LC-MS/MS was established.Samples of pig urine were diluted with ultra pure water,cleaned with immunoaffinity chromatography column,and then eluted with the methyl alcohol.The elution was then filtered through the 0.22 μm organic needles filter and seperated using liquid chromatography separation.Then the samples were ionized using electricity atomization ion aource ionization,and examined using the ion monitor（MRM） and quantified by external standard method.Using 0.1% formic acid： the methyl cyanide ＋ methyl alcohol solution（1＋1） as mobile phase,gradient elution,and 0.3 mL/min flow rate.The good linearity was in the range of 0.01 μg/kg to 0.50 μg/kg.The limits of quantification was 0.01 μg/kg,and the corresponding recoveries was between 70%~95%,The method is simple,rapid,sensitive and accurate.It is suitable for the determination of aflatoxin M1 in pig urine.