同位素内标稀释-UPLC-MS/MS法同时测定生活饮用水中5种消毒副产物和高氯酸盐  

Simultaneous Determination of Five Disinfection Byproducts and Perchlorate in Drinking Water by Isotope Internal Standard Dilution UPLC-MS/MS Method

作　　者：侯婧 刘双德[1] HOU Jing;LIU Shuang-de(Qinghai Center for Disease Prevention and Control,Xining 810000,China)

机构地区：[1]青海省疾病预防控制中心,青海西宁810000

出　　处：《化学试剂》2025年第1期67-73,共7页Chemical Reagents

摘　　要：利用同位素稀释技术建立一种可同时测定生活饮用水中二氯乙酸、三氯乙酸、氯酸盐、亚氯酸盐和溴酸盐5种消毒副产物以及高氯酸盐的超高效液相色谱串联质谱(ID-UPLC-MS/MS)检测方法。样品过膜后加入同位素内标,采用Torus DEA色谱柱(100 mm×2.1 mm,1.7μm)分离,以0.5%氨水-1 mmol/L乙酸铵和乙腈为流动相洗脱,多反应监测(MRM)负模式(ESI-)测定,内标法定量。6种化合物线性相关系数r均大于0.990,检出限为1.5~2.1μg/L,定量限为5.0~7.0μg/L,应用该方法对399份水样进行测定,检出率为16.04%。该方法采用同位素内标稀释直接进样,分析速度快,灵敏度高,数据准确适用于饮用水国家标准(GB/T 5750.5—2023和GB/T 5750.10—2023)检测限值的要求。An isotope dilution technique coupled with ultra-performance liquid chromatography-tandem mass spectrometry(ID-UPLC-MS/MS)method was established for simultaneous determination of disinfection byproducts such as dichloroacetic acid,trichloroacetic acid,chlorate,chlorite,bromate,and perchlorate in drinking water.The samples were separated by Torus DEA column(100 mm×2.1 mm,1.7μm),eluted with 0.5% ammonia-1 mmol/L ammonium acetate and acetonitrile as mobile phases,determined by multiple reaction monitoring(MRM)negative mode(ESI-),and quantified by internal standard method.The linear correlation coefficients for all six compounds were greater than 0.990.The detection limits was 1.5~2.1μg/L,and the quantitation limits was 5.0~7.0μg/L.The detection rate was 16.04% in 399 water samples.The method involves direct injection of samples using isotope internal standard dilution,resulting in fast analysis speed,high sensitivity,and accurate data.This method is suitable for detecting compounds within the limits set by the drinking water national standards(GB/T 5750.5—2023 and GB/T 5750.10—2023).

关 键 词：生活饮用水 超高效液相色谱串联质谱法 消毒副产物 高氯酸盐 Torus DEA色谱柱 同位素内标稀释 

分 类 号：O657.63[理学—分析化学]