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建立了一种采用同位素稀释-液相色谱-串联质谱同时快速测定婴幼儿米粉中的三聚氰胺和丙烯酰胺含量的方法。样品经甲醇水溶液超声提取,浓缩吹干后用流动相溶解定容后,采用电喷雾串联质谱进行定性和定量分析。结果表明,其两种化合物的质量浓度与其峰面积在一定范围内均呈线性关系,线性相关系数大于0.99,三聚氰胺的方法检出限(3S/N)为3μg.kg-1,丙烯酰胺的方法检出限(3S/N)为15μg.kg-1,测得加标回收率在89.4%～93.4%之间,相对标准偏差在3.68%～6.36%之间。该方法具有前处理简单、灵敏度高的优点,适用于婴幼儿米粉中三聚氰胺和丙烯酰胺的定性确认和定量检测。
A rapid method for the simultaneous determination of melamine and acrylamide in infant rice flour by isotope dilution-liquid chromatography-tandem mass spectrometry was established. The sample was extracted by methanol aqueous solution, concentrated and dried, and then dissolved and fixed in mobile phase. Qualitative and quantitative analysis was carried out by electrospray tandem mass spectrometry. The results showed that the mass concentration of the two compounds showed a linear relationship with the peak area within a certain range, the linear correlation coefficient was greater than 0.99, the detection limit (3S / N) of melamine was 3μg.kg-1, acrylamide method The detection limit (3S / N) was 15μg.kg-1. The spiked recoveries ranged from 89.4% to 93.4% with relative standard deviations between 3.68% and 6.36%. The method has the advantages of simple pretreatment and high sensitivity, and is suitable for qualitative confirmation and quantitative detection of melamine and acrylamide in infant rice flour.