生活饮用水中卤乙酸和卤氧化物离子色谱-串联质谱的同时测定法  

Simultaneous determination of haloacetic acid and oxyhalide in drinking water by ion chromatography-tandem mass spectrometry

作　　者：白丝雨 王硕[1] 孙灵利[1] BAI Si-yu;WANG Shuo;SUN Ling-li(Physical and Chemical Laboratory,Chaoyang District Center for Disease Control and Prevention,Beijing,100021,China)

机构地区：[1]北京市朝阳区疾病预防控制中心理化检验科,北京100021

出　　处：《职业与健康》2021年第20期2757-2760,共4页Occupation and Health

基　　金：2022年冬奥会突发公共卫生事件应急保障技术平台建设项目(CYSF2011)。

摘　　要：目的建立测定生活饮用水中卤乙酸和卤氧化物的离子色谱-串联质谱法。方法样品经过0.2μm的滤膜后待测,经烷醇季胺型离子交换柱DionexIonPacTMAS19分析柱(2×250 mm)分离,使用乙腈作为流动相,KOH梯度洗脱,采用电喷雾离子源(ESI-),多反应离子检测(MRM)模式,负离子模式为扫描模式,经离子色谱电导检测器后连接三重四极质谱进行检测,根据被测物的保留时间和特征离子峰进行定量分析,用外标法和内标法进行定量分析。结果3种卤乙酸(二氯乙酸、三氯乙酸、碘乙酸)和3种卤氧化物(溴酸盐、氯酸盐、亚氯酸盐)在0.5~400.0μg/L范围内呈现出良好的线性关系,相关系数r>0.992,检出限为0.06~0.75μg/L,定量限为0.2~2.5μg/L。在生活饮用水中分别进行低、中、高浓度的加标回收实验,回收率为79.3%~121.0%,相对标准偏差(RSD)为1.25%~8.53%。应用本方法对朝阳地区生活饮用水中卤乙酸和卤氧化物浓度进行检测,检出二氯乙酸浓度为0.3~1.1μg/L,三氯乙酸浓度为5.9~26.2μg/L,溴酸盐浓度为0.7~174.0μg/L,氯酸盐浓度为141~240μg/L,亚氯酸盐和碘乙酸均未检出。结论该方法快捷简便,灵敏准确,可用于生活饮用水中卤乙酸、溴酸盐、氯酸盐和亚氯酸盐的日常检测工作。Objective To establish an ion chromatography-tandem mass spectrometry method for the determination of haloacetic acid and oxyhalide in drinking water.Methods The sample wasto be tested after passing through a 0.2μm filter membrane,and was separated by an alkanol quaternary ammonium ion exchange column DionexIonPac;AS19 analytical column(2×250 mm),with acetonitrile as the mobile phase and KOH gradient elution.Using electrospray ion source(ESI-),multiple reactive ion detection(MRM)mode,and the negative ion scanning mode,the ion chromatography conductivity detector connected to the triple quadrupole mass spectrometer was used for detection.The quantitative analysis was performed according to the retention time of the analyte and the characteristic ion peak,and the external standard method and internal standard method was used for quantitative analysis.Results Three kinds of haloacetic acids(dichloroacetic acid,trichloroacetic acid,iodoacetic acid)and three kinds of oxyhalides(bromate,chlorate,chlorite)showed a good linear relationship in the range of 0.5-400.0μg/L,and the correlation coefficient(r)was>0.992.The detection limits were 0.06-0.75μg/L,and the quantification limits was 0.2-2.5μg/L.Low,medium and high concentration recovery experiments were carried out in drinking water,the recovery rate was 79.3%-121.0%,and the relative standard deviation(RSD)was 1.25%-8.53%.This method was used to detect haloacetic acid and oxyhalide in drinking water in Chaoyang area,and the results were as follows:dichloroacetic acid concentration was 0.3-1.1μg/L,trichloroacetic acid concentration was 5.9-26.2μg/L,bromate concentration was 0.7-174.0μg/L,chlorate concentration was 141-240μg/L,while chlorite and iodoacetic acid were not detected.Conclusion The method is quick,simple,sensitive and accurate,and can be used for daily detection of haloacetic acid,bromate,chlorate and chlorite in drinking water.

关 键 词：卤乙酸 卤氧化物 生活饮用水 离子色谱-串联质谱 

分 类 号：R115[医药卫生—公共卫生与预防医学]