饮用水中丙烯酰胺的测定及不确定度评定  

Determination of acrylamide in drinking water and uncertainty evaluation

作　　者：陈东洋[1] 张昊[1] 冯家力[1] 曾栋[1] 王一红[1] 李帮锐[1] 刘先军[1] CHEN Dong-yang;ZHANG Hao;FENG Jia-li;ZENG Dong;WANG Yi-hong;LI Bang-rui;LIU Xian-jun(Physical and Chemical Laboratory,HuMan Provincial Center for Disease Control and Prevention,Changsha HuMan,410005,China)

机构地区：[1]湖南省疾病预防控制中心理化检验科,湖南长沙410005

出　　处：《职业与健康》2018年第22期3063-3067,共5页Occupation and Health

基　　金：2013年卫生标准制修订计划项目(20130106)

摘　　要：目的建立饮用水中痕量丙烯酰胺的高效液相色谱-串联质谱法的测定方法,并对该方法进行不确定度评定,分析不确定度来源,计算各不确定分量。方法样品通过活性炭固相萃取柱富集,甲醇洗脱,采用反相C18色谱柱分离,以甲醇-0.1%甲酸水溶液作为流动相,以选择反应监测(SRM),ESI+电离方式,内标法定量。不确定度评定则按照JJF 1059.1-2012《测量不确定度评定与表示》对该方法进行A类不确定度评定。结果丙烯酰胺在1.0~100.0μg/L浓度范围内,相关系数为0.999 5,RSD≤5.1%,回收率为96.1%~99.8%,若取100 ml水样测定,检出限为0.005μg/L。结论评定结果表明,标准溶液配制和重复性测定是不确定度的主要来源。该方法快速,准确,灵敏度,适用于饮用水中丙烯酰胺的测定。[Objective ] To develop a method based on liquid chromatography coupled to tandem mass spectrometry （LC-MS/MS） for the determination of trace acrylamide in drinking water, evaluate the uncertainty of the method, analyze the sources of uncertainty and calculate the uncertain components. [Methods] The samples were enriched by activated carbon solid phase extraction column, eluted by methanol and separated by reversed phase C18 column with a mobile phase consisting of methanol and 0.1% formic acid. The MS/MS detection was performed under the select reaction monitoring （SRM） mode via positive electrospray ionization（ESI＋）, and the internal standard method was used for the quantitative analysis. According to Evaluation and Representation of Uncertainty in Measurement （JJF 1059.1-2012）, the class A uncertainty evaluation was conducted. [Results] In the acrylamide concentration range of 1.0-100.0 μg/L, the correlation coefficient was 0.999 5, RSD≤5.1%, and recoveries were 96.1%-99.8%. The limit of detection was 0.005 μg/L with 100 injection volume of water sample. [Conclusion] The evaluation results showed that the major sources of uncertainty in determination are standard solution preparation and repeatability. The method is fast, accurate and sensitive, and is suitable for the determination of acrylamide in drinking water.

关 键 词：丙烯酰胺 固相萃取 高效液相色谱-串联质谱法 不确定度 

分 类 号：R123.1[医药卫生—环境卫生学]