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目的采用同位素稀释-超高效液相色谱-串联质谱法测定婴幼儿谷物米粉中伏马菌素B_1、B_2及B_3含量。方法样品经乙腈-水溶液(30∶70,V/V)提取,MultiSep 211Fum净化柱净化,采用ZORBAXSB-C_(18)色谱柱分离,以乙腈和水(含0.1%甲酸)为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式检测,同位素内标法定量。结果伏马菌素B1、B2及B3的浓度为5μg/L~1 000μg/L时,线性关系良好,相关系数(r)>0.999。添加10μg/kg、50μg/kg、100μg/kg 3个不同水平时,伏马菌素B的回收率为76.8%~90.1%,精密度RSD为3.7%~9.0%,检出限为0.5μg/kg。结论该方法的灵敏度及准确度良好,可应用于日常大批量样品的高灵敏分析。
Objective To determine the contents of fumonisin B_1, B_2 and B_3 in infant cereal rice by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile-water (30:70, V / V), cleaned up with MultiSep 211Fum column and separated on a ZORBAXSB-C 18 column. The mobile phase consisted of acetonitrile and water containing 0.1% formic acid Off, using electrospray - positive ion multi-reaction monitoring mode detection, isotope internal standard method. Results When the concentration of fumonisin B1, B2 and B3 was 5μg / L ~ 1 000μg / L, the linear relationship was good with the correlation coefficient (r)> 0.999. The recoveries of fumonisin B were 76.8% -90.1% with RSD of 3.7% -9.0 at 3 μg / kg, 10 μg / kg, 50 μg / kg and 100 μg / kg with the detection limit of 0.5 μg / kg. Conclusion The sensitivity and accuracy of the method are good and can be applied to the high sensitive analysis of daily large batch samples.