UPLC-MS/MS测定液体乳中氯酸盐和高氯酸盐的不确定度评定  

Uncertainty Assessment for Determination of Chlorate and Perchlorate in Liquid Milk by UPLC-MS/MS

作　　者：苏阿龙 侯莉莉 周佳 杨振东 文树新 SU Along;HOU Lili;ZHOU Jia;YANG Zhendong;WEN Shuxin(Gansu Food Inspection and Research Institute,Lanzhou 730300,China)

机构地区：[1]甘肃省食品检验研究院,甘肃兰州730300

出　　处：《食品安全导刊》2024年第11期67-71,共5页China Food Safety Magazine

基　　金：市场监管总局科技计划项目(2022MK127)。

摘　　要：目的:评定UPLC-MS/MS测定液体乳中氯酸盐和高氯酸盐的不确定度。方法:依据国家标准GB 5009.291—2023对液体乳制品中氯酸盐、高氯酸盐测定过程不确定度的各影响因子进行分析,建立数学模型对不确定度各分量进行量化,全面分析不确定度的来源并进行计算。结果:测得的液体乳中氯酸盐含量为30.4 μg·kg^(-1),扩展不确定度为3.7 μg·kg^(-1),k=2;高氯酸盐含量为40.3 μg·kg^(-1),扩展不确定度为5.3 μg·kg^(-1),k=2。不确定度的来源主要是系列标准工作液的配制、待测样液的制备、仪器分析测试等。结论:该研究可以反映测量氯酸盐和高氯酸盐的置信度和准确度,为液体乳的检测提供有益参考。Objective:To evaluate the uncertainty of chlorate and perchlorate determination in liquid milk by UPLC-MS/MS.Method:According to the national standard GB 5009.291—2023,the influencing factors of the uncertainty of the determination process of chlorate and perchlorate in liquid dairy products were analyzed,and the mathematical models were established to quantify the uncertainty components,and the sources of uncertainty were comprehensively analyzed and calculated.Result:The measured chlorate content in liquid milk was 30.4μg·kg^(-1),with an expanded uncertainty of 3.7μg·kg^(-1),k=2;the perchlorate content was 40.3μg·kg^(-1),with an expanded uncertainty of 5.3μg·kg^(-1),k=2.The sources of uncertainty were mainly the preparation of the standard series,the preparation of the sample solution,and the instrumental analysis test.Conclusion:This study can reflect the confidence and accuracy of measuring chlorates and perchlorates,providing favorable references for the detection of liquid milk.

关 键 词：超高效液相色谱-串联质谱法 液体乳 氯酸盐 高氯酸盐 不确定度 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]