液相色谱-串联质谱法检测生活饮用水中氯酸盐、溴酸盐和亚氯酸盐  

Determination of chlorate,bromate,and chlorite in drinking water by liquid chromatography-tandem mass spectrometry

作　　者：邱凤梅[1] 方力[2] 邵诚杰 QIU Feng-mei;FANG Li;SHAO Cheng-jie(Daishan County Center for Disease Control and Prevention(Daishan County Food Inspection and Testing Center),Daishan,Zhejiang 316200,China;不详)

机构地区：[1]岱山县疾病预防控制中心(岱山县食品检验检测中心),浙江岱山316200 [2]浙江省海产品健康危害因素关键技术研究重点实验室(舟山市疾病预防控制中心),浙江舟山316021

出　　处：《中国卫生检验杂志》2022年第1期23-26,共4页Chinese Journal of Health Laboratory Technology

基　　金：舟山市公益类科技计划(2021C31071);舟山市医药卫生科技计划(2020YA01)。

摘　　要：目的建立生活饮用水中氯酸盐、溴酸盐和亚氯酸盐的液相色谱串-联质谱检测方法。方法水样经0.22μm亲水PTFE滤膜过滤后,采用Acclaim Trinity P1色谱柱分离,20 mmol/L甲酸铵和乙腈为流动相梯度洗脱,在电喷雾离子化(ESI-)、选择反应监测(SRM)模式下检测,外标法定量。结果氯酸盐、溴酸盐和亚氯酸盐的线性范围分别为0.20μg/L~20.0μg/L、1.0μg/L~100.0μg/L和20.0μg/L~1 000μg/L,相关系数达到0.999以上;方法检出限分别为0.06μg/L、0.30μg/L和6.0μg/L,方法定量限分别为0.20μg/L、1.0μg/L和20.0μg/L;在低、中、高3个浓度水平下加标,氯酸盐、溴酸盐和亚氯酸盐的回收率分别为89.7%~92.7%、94.4%~108.1%和89.0%~100.1%,日内与日间相对标准偏差(RSD)分别为1.0%~7.4%和0.8%~8.0%。结论该方法准确、快速、易操作,能满足饮用水中氯酸盐、溴酸盐和亚氯酸盐的日常检测要求。Objective A liquid chromatography-tandem mass spectrometry for quantitative analysis of chlorate, bromate, and chlorite in drinking water was established.Methods The water sample was filtered through a 0. 22 μm PTFE filter membrane and then the analytes were separated on an Acclaim Trinity P1 column with mobile phases of 20 mmol/L ammonium formate and acetonitrile, and detected in selected reaction monitoring(SRM) mode via negative electrospray ionization. The external standard method was used for quantitation.Results The linear ranges of chlorate, bromate, and chlorite were within 0. 20 μg/L-20. 0 μg/L, 1. 0 μg/L-100. 0 μg/L, and 20. 0 μg/L-1 000 μg/L, respectively, with the correlation coefficients higher than0. 999. The detection limits of chlorate, bromate, and chlorite were 0. 06 μg/L, 0. 30 μg/L, and 6. 0 μg/L, respectively, and the quantification limits were 0. 20 μg/L, 1. 0 μg/L, and 20. 0 μg/L, respectively. The recoveries of chlorate, bromate, and chlorite at three spiking levels were 89. 7%-92. 7%, 94. 4%-108. 1%, 89. 0%-100. 1%, respectively. The inter-and intra-dayRSDswere 1. 0%-7. 4% and 0. 8%-8. 0%.Conclusion The method is accurate, fast, easy to operate, which can satisfy the requirements of routine analysis.

关 键 词：氯酸盐 溴酸盐 亚氯酸盐 消毒副产物 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]