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建立了免疫亲和层析净化同时测定生鲜乳中黄曲霉毒素M_1和M_2的-超高效液相色谱(ultra high performance liquid chromatography,UHPLC)-荧光检测法。黄曲霉毒素M_1仪器线性范围0.40~100μg/mL,仪器定量限0.40 ng/mL,仪器检出限0.10 ng/mL,方法检出限0.005μg/kg,回收率91.8%~96.8%;。黄曲霉毒素M_2仪器线性范围0.10~100μg/mL,仪器定量限0.10 ng/mL,仪器检出限0.03 ng/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M_1的风险是安全可控的。此外除了黄曲霉毒素M_1,还应加强黄曲霉毒素M_2的监控。
An ultra-high performance liquid chromatography (UHPLC)-fluorescence method was developed for the simultaneous determination of aflatoxins M_1 and M_2 in fresh milk by immunoaffinity chromatography. The linear range of aflatoxin M_1 was 0.40 ~ 100μg / mL, the limit of detection was 0.40 ng / mL. The detection limit was 0.10 ng / mL. The detection limit was 0.005 μg / kg. The recoveries ranged from 91.8% to 96.8%. The linear range of aflatoxin M_2 was 0.10 ~ 100μg / mL. The limit of quantification was 0.10 ng / mL. The detection limit was 0.03 ng / mL. The detection limit was 0.0015 μg / kg. The recoveries ranged from 86.4 to 94.1%. Both the intra-and inter-day CVs were less than 10%. Using this method, 20 fresh milk samples from 20 pastures in Chengdu were determined. As a result, the risk of aflatoxin M1 was safely and controllable. In addition to aflatoxin M_1, should also be strengthened aflatoxin M_2 monitoring.