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)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。
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.
作者
詹胜群
张浩
周钧
葛城
刘金梅
周荣杰
储晓刚
刘倩
ZHAN Shengqun;ZHANG Hao;ZHOU Jun;GE Cheng;LIU Jinmei;ZHOU Rongjie;CHU Xiaogang;LIU Qian(Ausnutria Dairy(China)Co.,Ltd.,Changsha 410200,China)
出处
《食品科技》
CAS
北大核心
2022年第1期312-318,共7页
Food Science and Technology
作者简介
詹胜群,男,研究方向为食品安全与检验;通信作者:刘倩。
