建立了免疫亲和层析净化同时测定生鲜乳中黄曲霉毒素M1和M2的-超高效液相色谱(ultra high performance liquid chromatography, UHPLC)-荧光检测法。黄曲霉毒素M1仪器线性范围0.40~100μg/mL,仪器定量限0.40ng/mL,仪器检出限0.10ng/mL,方法检出FK0.005μg/kg,回收率91.8%~96.8%;。黄曲霉毒素M2仪器线性范围0.10~100μ/mL,仪器定量限0.10ng/mL,仪器检出限0.03ng/mL,方法检出限0.0015μg/kg,回收率86.4至94.1%。两者的日内和日间变异系数均小于10%。使用该方法对来自成都市20个牧场的20个生鲜乳进行了测定,结果黄曲霉毒素M1的风险是安全可控的。此外除了黄曲霉毒素M1,还应加强黄曲霉毒素M2的监控。
An ultra high performance liquid chromatography with fluorescence detection (UHPLC-FLD) after immunoaffinity column puri- fication has been developed for the simultaneous determination of AFM1 and AFM2 in raw milk. The linear range of AFM1 is 0.40-100 p,g/ mL and the instrumental limits of quantification and determination are 0.40 ng/mL and 0.10 ng/mL, respectively. The limit of determination of method is 0.005 μg/kg and the average recoveries were 91.8%-96.8% for AFM1. The hnear range of AFM2 is 0.10-100 μg/mL and the instrumental limits of quantification and determination are 0.10 ng/mL and 0.03 ng/mL, respectively. The limit of determination of method is 0.0015 μg/kg and the average recoveries were 86.4%-94.1% for AFM2. Inter and intra day CVs were lower than 10% for both AFM1 and AFM2. The proposed sensitive UHPLC-FLD method was applied to 20 raw milk samples collected from 20 different pastures in Chengdu. As the results indicate, the contamination level of AFM1 is quite safe. Besides, AFM2 should also be routinely monitored along with AFM1.