超高效液相色谱-串联质谱测定水源水中176种药品和个人护理用品含量  

Determination of the Concentrations of 176 Pharmaceutical and Personal Care Products in Drinking Water Samples by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吴少明 刘文菁 戴明 何孟杭 陈言凯 王征 詹重清 欧阳立群 WU Shaoming;LIU Wenjing;DAI Ming;HE Menghang;CHEN Yankai;WANG Zheng;ZHAN Chongqing;OUYANG Liqun(Fujian Inspection and Research Institute for Product Quality,National Quality Supervision and Testing Center for Processed Food,Fuzhou 350002,China)

机构地区：[1]福建省产品质量检验研究院,国家加工食品质量检验检测中心,福建福州350002

出　　处：《食品科学》2024年第4期307-314,共8页Food Science

基　　金：市场监管总局科技计划资助项目(2021MK054)。

摘　　要：基于固相萃取结合超高效液相色谱-串联质谱技术建立同时测定水源水中176种药品和个人护理用品(pharmaceutical and personal care products,PPCPs)含量的方法。将水源水调节至pH 7后,经Cleanert PEP固相萃取柱富集净化,洗脱液采用二甲基亚砜辅助浓缩后,以甲醇-0.1%甲酸水(含0.2 mmol乙酸铵)为流动相,在HSS T3色谱柱(2.1 mm×150 mm,1.8μm)中进行分离,用电喷雾离子源(正负离子切换模式)、多反应监测模式进行测定。方法学验证结果表明,176种PPCPs在5~200 ng/mL范围内线性关系较好,相关系数均高于0.99。176种PPCPs的方法的定量限为0.1 ng/mL。在空白水样中进行3种加标水平(0.1、0.4、1.0 ng/mL)的加标回收实验(n=6),176种化合物的平均回收率在68.0%~126.7%之间,相对标准偏差在1.1%~10.3%之间。综上,本研究所建立的方法简单快速、重现性好、灵敏度高,能够满足水源水中176种PPCPs含量的高通量检测要求。A method for simultaneous determination of 176 pharmaceuticals and personal care products(PPCPs)in drinking water samples was established by combining solid-phase extraction(SPE)with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The water samples were adjusted to pH 7,and then subjected to enrichment and purification using a Cleanert PEP SPE column.After concentration of the eluate with dimethyl sulfoxide(DMSO),the chromatographic separation was carried out on an HSS T3 column(2.1 mm×150 mm,1.8μm)using methanol-0.1%formic acid water(containing 0.2 mmol ammonium acetate)as the mobile phase.The detection was performed in positive and negative ionization switching modes with multiple reaction monitoring(MRM).Methodological validation results showed that good linearity for the 176 PPCPs was achieved in the concentration range of 5–200 ng/mL,with a correlation coefficient higher than 0.99.The limit of quantitation(LOQ)of the method for all the PPCPs was 0.1 ng/mL.The average recoveries of spiked blank samples at three levels(0.1,0.4 and 1.0 ng/mL)were between 68.0%and 126.7%,with relative standard deviation(RSD)between 1.1%and 10.3%(n=6).In conclusion,the method established in this study is simple,rapid,reproducible,and highly sensitive,and can meet the requirements of the high-throughput detection of the 176 PPCPs in drinking water sources.

关 键 词：固相萃取 超高效液相色谱-串联质谱 药品和个人护理用品 水源水 

分 类 号：TS207.3[轻工技术与工程—食品科学]