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激光二极管热解吸/常压化学电离串联质谱法分析废水中选定的甾体激素:方法优化与应用。

Laser diode thermal desorption/atmospheric pressure chemical ionization tandem mass spectrometry analysis of selected steroid hormones in wastewater: method optimization and application.

机构信息

Department of Chemistry, Université de Montréal, Quebec, Canada.

出版信息

Anal Chem. 2010 Jan 15;82(2):639-45. doi: 10.1021/ac902074x.

DOI:10.1021/ac902074x
PMID:20000768
Abstract

A rapid and reliable method enabling high-throughput sample analysis for quicker data generation, detection, and monitoring of eight selected steroid hormones in water matrixes was developed and validated. Our approach is based on a novel sample introduction method, the laser diode thermal desorption/atmospheric pressure chemical ionization (LDTD/APCI) coupled to tandem mass spectrometry (MS/MS). The optimization of instrumental parameters and a method application are presented. Our method was successfully applied to spiked effluent wastewater in the low-nanogram per liter concentrations with total analysis time reduced to seconds (15 s) using LDTD/APCI-MS/MS compared to minutes with traditional liquid-chromatography coupled to tandem mass spectrometry (LC-MS/MS) following solid-phase extraction (SPE). The instrumental detection limits for LDTD/APCI-MS/MS ranged from 5 to 24 microg L(-1) and from 13 to 43 ng L(-1) for the method detection limits. Calibration curves in wastewater matrix showed good linearity (R(2) > 0.99), and precision (intraday and interday) was below 20%. This work demonstrates that LDTD/APCI-MS/MS could be used for fast and effective quantitative analysis of emerging contaminants in different water matrixes with reduced cost by eliminating the chromatography step used in traditional LC-MS/MS.

摘要

建立并验证了一种快速可靠的方法,可实现高通量样品分析,从而更快地生成、检测和监测水基质中 8 种选定的甾体激素。我们的方法基于一种新颖的样品引入方法,即激光二极管热解吸/常压化学电离(LDTD/APCI)与串联质谱(MS/MS)相结合。本文介绍了仪器参数的优化和方法应用。与传统的固相萃取(SPE)后液相色谱-串联质谱(LC-MS/MS)相比,本方法将总分析时间从数分钟缩短至 15 秒,成功应用于低纳克每升浓度的加标废水。与 LC-MS/MS 相比,LDTD/APCI-MS/MS 的仪器检测限范围为 5 至 24 微克/升,方法检测限范围为 13 至 43 纳克/升。废水基质中的校准曲线具有良好的线性(R(2)>0.99),日内和日间精密度均低于 20%。本工作表明,通过消除传统 LC-MS/MS 中使用的色谱步骤,LDTD/APCI-MS/MS 可用于快速有效地定量分析不同水基质中的新兴污染物,同时降低成本。

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