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    在线固相萃取-超高效液相色谱-串联质谱法测定水源水和饮用水中50种药品和个人护理品及其代谢物的含量

    Determination of 50 Pharmaceuticals and Personal Care Products and Their Metabolites in Raw Water and Drinking Water by Online Solid Phase Extraction-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 为降低水样及有机试剂用量、简化前处理流程,采用题示方法测定水源水和饮用水中50种药品和个人护理品(PPCPs)及其代谢物的含量。采集水样,每升水样加入30 mg抗坏血酸,分取20 mL过0.22 µm聚四氟乙烯滤膜,收集滤液,用甲酸调节其酸度至pH 2~3,加入100 μg·L−1混合内标溶液10 μL,分取5 mL进入在线双固相萃取系统,在XBridge C18在线固相萃取柱上进行净化和富集,然后通过阀切换将所得溶液引入超高效液相色谱-串联质谱系统,50种目标物在Waters ACQUITY UPLC BEH C18 色谱柱上以0.1%(体积分数)甲酸溶液-甲醇体系进行梯度洗脱分离,在电喷雾离子源正离子和多反应监测模式下进行内标法定量。结果显示,50种目标物的质量浓度均在一定范围内和目标物与内标的定量离子峰面积比值呈线性关系,检出限为0.01~1.00 ng·L−1。按照标准加入法进行回收试验,回收率为61.9%~133%,测定值的相对标准偏差(n=6)不大于25%。方法用于46份水样的分析,检出了磺胺氯哒嗪、磺胺二甲基嘧啶、磺胺吡啶、磺胺甲唑、1,7-二甲基黄嘌呤、对乙酰氨基酚、卡马西平,检出量为1.99~66.20 ng·L−1

       

      Abstract: To reduce the consumption of water samples and organic reagents and simplify the pretreatment process, the method mentioned by the title was employed to determine 50 pharmaceuticals and personal care products (PPCPs) and their metabolites in raw water and drinking water. Water samples were collected, and 30 mg of ascorbic acid was added per liter of water sample. An aliquot (20 mL) was taken, and passed through a 0.22 µm polytetrafluoroethylene filter membrane. The filtrate was collected, and its acidity was adjusted to pH 2-3 with formic acid, followed by addition of 10 μL of 100 μg·L−1 mixed internal standard solution. An aliquot (5 mL) was taken, and introduced into the online dual solid phase extraction system for purification and enrichment on XBridge C18 online solid phase extraction column. The resulting solution was then transferred via valve switching to the ultra-high performance liquid chromatography-tandem mass spectrometry system. The 50 target compounds were separated on Waters ACQUITY UPLC BEH C18 column using a gradient elution system consisting of 0.1% (volume fraction) formic acid solution and methanol. Quantification was performed in modes of positive electrospray ionization and multiple reaction monitoring using the internal standard method. It was shown that linear relationships between the mass concentrations of 50 target compounds and peak area ratios of target compounds to internal standards were kept in definite ranges, with detection limits in the range of 0.01-1.00 ng·L−1. Test for recovery was made by the standard addition method, giving recoveries in the range of 61.9%-133%, and RSDs (n=6) of the determined values did not exceed 25%. The proposed method was applied to the analysis of 46 water samples, sulfachloropyridazine, sulfamethazine, sulfapyridine, sulfamethoxazole, 1,7-dimethylxanthine, paracetamol, and carbamazepine were detected at detection amounts in the range of 1.99-66.20 ng·L−1.

       

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