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采用在线自动化固相萃取-液相色谱-串联质谱法(SPE-LC-MS/MS)测定环境水样中的 19 种磺胺类药物。

Determination of 19 sulfonamides in environmental water samples by automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS).

机构信息

Department of Environmental Chemistry, Institute of Environmental Assessment and Water Studies (IDAEA), Spanish Council of Scientific Research (CSIC), Jordi Girona 18-26, E-08034 Barcelona, Spain.

出版信息

Talanta. 2010 Apr 15;81(1-2):355-66. doi: 10.1016/j.talanta.2009.12.009. Epub 2009 Dec 16.

Abstract

The present study describes the development, validation and a practical application of a fully automated analytical method based on on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) for the simultaneous determination of 19 sulfonamides, including one acetylated metabolite, in different water matrices. MS/MS detection was carried out in a quadrupole-linear ion trap (QqLIT) mass analyzer. Target compounds were identified in the selected reaction monitoring (SRM) mode, recording two transitions between precursor ions and the two most abundant product ions. The method developed was applied to evaluate the occurrence of the target antibiotics in different water samples: influent and effluent water from waste water treatment plants (WWTP), ground water and surface water. Under optimal conditions, the method detection limits achieved were in the range 0.05-7.84 ng/L for WWTP influent water, 0.01-6.90 ng/L for WWTP effluent water, 0.02-5.13 ng/L for ground water and 0.02-4.52 ng/L for surface water samples. The instrumental repeatability, expressed as RSD, was usually below 10% for the different water matrices. Results showed the wide presence of sulfonamides in the four types of water, including one acetylated metabolite, with maximum concentrations up to 855 ng/L corresponding to sulfapyridine in an influent waste water sample near a densely populated urban area.

摘要

本研究描述了一种基于在线固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)的全自动分析方法的开发、验证和实际应用,用于同时测定不同水基质中 19 种磺胺类药物,包括一种乙酰化代谢物。MS/MS 检测在四极杆-线性离子阱(QqLIT)质谱分析仪中进行。目标化合物在选择反应监测(SRM)模式下进行鉴定,记录前体离子和两个最丰富的产物离子之间的两个跃迁。所开发的方法用于评估目标抗生素在不同水样中的存在情况:废水处理厂(WWTP)的进水和出水、地下水和地表水。在最佳条件下,该方法的检测限在 WWTP 进水 0.05-7.84ng/L、WWTP 出水 0.01-6.90ng/L、地下水 0.02-5.13ng/L 和地表水 0.02-4.52ng/L 范围内。不同水基质的仪器重复性(以 RSD 表示)通常低于 10%。结果表明,磺胺类药物广泛存在于四种类型的水中,包括一种乙酰化代谢物,在人口稠密的城市地区附近的一个废水进水样本中,最高浓度可达 855ng/L,对应磺胺嘧啶。

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