超高效液相色谱-串联质谱法测定婴幼儿配方奶粉中的高氯酸盐和氯酸盐残留

Determination of perchlorate and chlorate residues in infant formula milk powder by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  婴幼儿配方奶粉  高氯酸盐  氯酸盐

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  infant formula milk powder  perchlorate  chlorate

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速测定婴幼儿配方奶粉中高氯酸盐和氯酸盐残留量的分析方法。方法 样品经乙腈提取后, 再经乙腈饱和的正己烷净化, Acclaim TRINITYP1复合色谱柱(50 mm×2.1 mm, 3 μm)进行分离。高氯酸盐和氯酸盐在优化后的色谱及质谱条件下, 采用负离子模式进行电离, 通过多反应监测(multiple reaction monitoring, MRM)模式对目标化合物进行测定, 使用内标法定量。结果 高氯酸盐和氯酸盐在各自线性范围内线性关系良好, 所得校准曲线线性相关系数均在0.999以上, 且精密度实验结果良好, 加标回收率在87.9%~109.5%之间。结论 本方法可以应用于婴幼儿配方奶粉中高氯酸盐和氯酸盐残留量的快速测定, 结果准确、可靠。

英文摘要:

      Objective To establish a method for the rapid determination of perchlorate and chlorate in infant formula milk powder by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with acetonitrile, purified with n-hexane saturated with acetonitrile, and purified with Acclaim TRINITYP1 composite chromatographic column (50 mm×2.1 mm, 3 μm) separate. Perchlorate and chlorate were ionized by negative ion mode under the optimized chromatographic and mass spectrometry conditions. The target compounds were determined by multiple reaction monitoring (MRM) mode and quantified by internal standard method. Results The linear relationship between perchlorate and chlorate in their respective linear range was good, the linear correlation coefficients of the calibration curves were more than 0.999, and the precision experimental results were good, and the recoveries of standard addition were between 87.9%?109.5%. Conclusion The method can be applied to the rapid determination of perchlorate and chlorate residues in infant formula milk powder with accurate and reliable results.