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高效液相色谱-串联质谱法同时测定地表水中33种药物
Simultaneous Determination of 33 Pharmaceuticals in Surface Water Using Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry
投稿时间:2022-05-13  修订日期:2023-05-30
DOI:10.19316/j.issn.1002-6002.2023.05.21
中文关键词:  固相萃取  高效液相色谱串联质谱  药物  地表水
英文关键词:solid phase extraction  high performance liquid chromatography tandem mass spectrometry  pharmaceuticals  surface water
基金项目:国家自然科学基金资助项目(42277406);国家重点研发计划项目(2017YFC0504401);中央高校基本科研业务费专项资助项目(2022YJSHH18)
作者单位
李庆山 中国矿业大学(北京)化学与环境工程学院, 北京 100083 
卜庆伟* 中国矿业大学(北京)化学与环境工程学院, 北京 100083 
曹红梅 中国矿业大学(北京)化学与环境工程学院, 北京 100083 
洪宸 中国矿业大学(北京)化学与环境工程学院, 北京 100083 
吴晓泽 中国矿业大学(北京)化学与环境工程学院, 北京 100083 
郭亚丽 中国矿业大学(北京)化学与环境工程学院, 北京 100083 
姜巍巍 上海城市水资源开发利用国家工程中心有限公司, 上海 200082 
通讯作者:卜庆伟*  中国矿业大学(北京)化学与环境工程学院, 北京 100083  
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中文摘要:
      采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)建立了地表水中25种抗生素类药物和8种非抗生素类药物的分析方法。通过重点优化质谱参数、色谱条件、样品pH、洗脱溶剂组成及用量等确定了最佳分析条件。水样经过滤、固相萃取柱富集净化后,选择Shim-pack XR-ODS为色谱柱,以乙腈和0.2%甲酸-2 mmol/L乙酸铵-水溶液为流动相进行梯度洗脱,采用电喷雾电离源,在多反应监测模式下(MRM)分析测定,内标法定量。33种药物的仪器定量限为0.012~4.68 ng/L,方法检出限为0.011~7.60 ng/L,地表水加标回收率为53.7%~122%,相对标准偏差为1.22%~32.1%(n=6)。方法成功应用于北京市凉水河12个地表水样分析,共检出32种药物,检出质量浓度为未检出~239 ng/L。利托那韦(RTV)作为新型冠状病毒诊疗方案中推荐的药物在凉水河检出率为100%。
英文摘要:
      An analytical method was developed for the determination of 25 antibiotics and 8 non-antibiotic pharmaceuticals in surface water by solid phase extraction coupled high performance liquid chromatography tandem mass spectrometry (SPE-HPLC-MS/MS). The optimum analytical conditions were determined by optimizing mass spectrometry parameters, chromatographic conditions, pH value of surface water samples, composition and volume of elute solvent. The water samples were filtrated and then enriched and cleaned up with SPE cartridges. The targeted pharmaceuticals were separated on a Shim-pack XR-ODS column by gradient elution with acetonitrile and 0.2% formic acid and 2 mmol/L ammonium acetate in water, and then analyzed with an electrospray ionization source and multiple reaction monitoring (MRM) mode. The pharmaceuticals were quantified by internal standard method. Instrument quantification limits and method detection limits for the 33 pharmaceuticals were 0.012-4.68 ng/L and 0.011-7.60 ng/L, respectively. The recovery rates of target pharmaceuticals at three spiked levels were 53.7%-122% with relative standard deviations of 1.22%-32.1%. Using the developed analytical method, 12 surface water samples in the Liangshui River of Beijing were analyzed. The results showed that 32 pharmaceuticals were detected and the concentrations were ND-239 ng/L. The detection rate of ritonavir (RTV) was 100% in the Liangshui River, which is a pharmaceutical against COVID-19 that was recommended by the National Health Commission of the People's Republic of China.
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