全自动固相萃取-液相色谱串联质谱法同时测定饮用水中21种有机磷酸酯及其代谢产物
Determination of 21 organophosphate esters and their metabolites in drinking water by automatic solid phase extraction-liquid chromatography-tandem mass spectrometry
袁蕊 1崔霞 2佟晶 1丁文波 1范赛2
作者信息
- 1. 北京市东城区疾病预防控制中心,北京 100050
- 2. 北京市疾病预防控制中心/北京市预防医学研究中心,北京 100013
- 折叠
摘要
目的 建立一种全自动固相萃取·液相色谱串联质谱法同时测定饮用水中21种有机磷酸酯(organophosphate esters,OPEs)及其代谢产物的方法.方法 饮用水加入内标后,采用HLB固相1萃取柱,全 自动固相萃取净化,甲醇洗脱,采用ACQUITY UPLC BEH(100 mm×2.1 mm,1.7 μm)色谱柱,液相色谱串联质谱法测定,内标法定量.结果 优化后的方法可以同时检测饮用水中21种有机磷酸酯及其代谢产物,检出限为0.01～0.24 ng/L,定量限为0.03～0.77 ng/L,加标0.8～20 ng/L,回收率范围为57.6％～121.2％,相对标准偏差为1.2％～11.1％(n=6).对17件市政末梢水及30件商超采集的包装饮用水进行测定,ΣOPEs范围为16.8～177ng/L,Σdi-OPEs范围为0.328～16.3 ng/L,说明水体存在有机磷酸酯及其代谢产物的暴露风险.结论 本法前处理自动化程度高、简单,灵敏度高,适用于大批量饮用水中有机磷酸酯及其代谢产物的同时高通量测定.
Abstract
OBJECTIVE To establish a method for simultaneous determination of 21 organophosphate esters(OPEs)and their metabolites in drinking water by automatic solid phase extraction-liquid chromatography-tandem mass spectrometry.METHODS The drinking water was purified by automatic solid phase extraction with HLB column,eluted by methanol,determined by liquid chromatography tandem mass spectrometry with ACQUITY UPLC BEH(100 mm×2.1 mm,1.7 μm)column,and quantified by internal standard method.RESULTS The optimized method could simultaneously detect 21 organophosphate esters and their metabolites in drinking water.The detection limit was 0.01-0.24 ng/L,the quantitation limit was 0.03-0.77 ng/L.The recovery range was 57.6％-121.2％and the relative standard deviation is 1.2％-11.1％when the concentration was 0.8-20 ng/L.Senventeen tap water and 30 packaged drinking water collected by the supermarket were measured.The ΣOPEs range was 16.8-177 ng/L,and the Σdi-OPEs range was 0.328-16.3 ng/L,indicating the exposure risk of organophosphates and their metabolites in water.CONCLUSION The pretreatment of the method is simple,automatic and sensitive,and is suitable for simultaneous high-throughput determination of organophosphate esters and their metabolites in large quantities of drinking water.
关键词
饮用水/有机磷酸酯/代谢产物/液相色谱-串联质谱Key words
drinking water/organophosphate esters/metabolites/liquid chromatography-mass spectrometry引用本文复制引用
基金项目
北京市东城区优秀人才培养项目(2021-dchrcprzz-44)
北京市东城区卫生科技计划(东卫健研[2023]-18)
出版年
2024
NETL
NSTL
维普
万方数据