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建立了用凝胶渗透色谱-超高效液相色谱/串联三重四级杆质谱测定牛奶中黄曲霉毒素M_1的方法。方法以乙腈超声提取,凝胶渗透色谱净化后,以乙腈-0.1%甲酸(3:7,V/V)为流动相,UPLC BEH C18分离,ESI+模式质谱检测,外标法定量。黄曲霉毒素M_1在0.1~4.0μg/L范围内线性关系良好,相关系数r为0.9955,检出限为0.01μg/kg,定量限为0.05μg/kg。牛奶样品在0.1,0.2,0.5μg/kg 3个加标浓度下,黄曲霉毒素M_1的回收率为72.4%~92.2%,相对标准偏差为4.0%~7.8%。
A method for the determination of aflatoxin M_1 in milk by gel permeation chromatography - ultra performance liquid chromatography / tandem triple quadrupole mass spectrometry was established. Methods The samples were eluted with acetonitrile and purified by gel permeation chromatography. The fractions were separated on a mobile phase of acetonitrile - 0.1% formic acid (3: 7, V / V), UPLC BEH C18 and ESI + mode. The linear relationship between aflatoxin M1 and 0.1 ~ 4.0μg / L was good with a correlation coefficient r of 0.9955, a detection limit of 0.01μg / kg and a limit of quantification of 0.05μg / kg. The recoveries of aflatoxins M_1 at 72 h, 72.2% and 90% relative standard deviations (RSDs) were 4.0% ~ 7.8% at the three spiked concentrations of 0.1, 0.2 and 0.5 μg / kg in milk samples respectively.