超高效液相色谱-串联质谱法测定婴幼儿配方乳粉中氯酸盐和高氯酸盐

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)同时测定婴幼儿配方乳粉中氯酸盐和高氯酸盐。方法:样品经过提取、离心、固相萃取柱净化和过滤,净化后滤液经负离子模式测定,并用内标法进行定量。结果:氯酸盐和高氯酸盐分别在2~500 μg/kg和1~250 μg/kg线性关系良好(R;>0.999),检出限均为4.5 μg/kg,定量限分别为15 μg/kg和7.5 μg/kg。对于方法正确度(n=9),在15.0、30.0 μg/kg和150 μg/kg 3个加标水平下,氯酸盐回收率为90.4%~104.3%;在7.5、15 μg/kg和75 μg/kg 3个加标水平下,高氯酸盐回收率为80.2%~106.2%。对于方法精密度(n=7),氯酸盐RSD为4.74%,高氯酸盐RSD为8.31%。结论:该方法线性、精密度和正确度数据均满足GB/T 27417—2017《化学分析方法确认和验证指南》的要求,适用于婴幼儿配方乳粉中氯酸盐和高氯酸盐的同时分析检测。

Determination of Chlorate and Perchlorate in Infant Formula Milk Powder by UPLC-MS/MS

Objective:To establish an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of chlorate and perchlorate in infant formula milk powder.Methods:The sample is extracted,centrifuged,purified and filtered by a solid phase extraction column.After purification,the filtrate is measured in the negative ion mode and quantified by the internal standard method.Results:Chlorate and perchlorate have a good linear relationship in the range of 2~500 μg/kg and 1~250 μg/kg respectively (R;>0.999),the detection limits are both 4.5 μg/kg,and the quantification limits are respectively 15,7.5 μg/kg.For accuracy (n=9),the chlorate recovery rate was 90.4%~104.3% at the three spike levels of 15.0,30.0,150 μg/kg;the three spikes at 7.5,15,75 μg/kg at the horizontal level,the recovery rate of perchlorate is 80.2%~106.2%.For method precision (n=7),the RSD of chlorate was 4.74% and the RSD of perchlorate was 8.31%.Conclusion:The linearity,precision and accuracy of this method meet the requirements of GB/T 27417—2017 “Guidelines for the Confirmation:and Verification of Chemical Analysis Methods”,and it is suitable for the simultaneous analysis of chlorate and perchlorate in infant formula milk powder detection.