Rapid automated screening, identification and quantification of organic micro-contaminants and their main transformation products in wastewater and river waters using liquid chromatography-quadrupole-time-of-flight mass spectrometry with an accurate-mass database
Rapid automated screening, identification and quantification of organic micro-contaminants and their main transformation products in wastewater and river waters using liquid chromatography-quadrupole-time-of-flight mass spectrometry with an accurate-mass database
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DOI：
10.1016/j.chroma.2010.08.070
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发表时间：
2010-11-05
影响因子：
4.1
通讯作者：
Fernandez-Alba, A. R.
中科院分区：
文献类型：
--
作者：
Gomez, M. J.;Gomez-Ramos, M. M.;Fernandez-Alba, A. R.
在这项研究中，我们开发和评估了一种快速自动筛选和确认大量有机微污染物的分析方法（近400个）以及对不同类型水样中阳性结果的量化使用液相色谱-电喷雾四极杆-飞行时间质谱法（LC-QTOFMS）基于使用精确质量数据库创建的数据库不仅包括关于目标离子的精确质量的数据，而且还包括关于源碎片离子同位素模式和保留时间数据该定制的数据库连接到商业上可获得的软件，该软件提取所有潜在的化合物从每个样品的LC-QTOFMS原始数据中提取感兴趣的化合物，并将其与数据库进行匹配，以搜索样品中的目标化合物。详细的碎片信息也被用作自动识别未知化合物的有力工具。或具有与数据库中包括的已知有机污染物的结构相似的结构的转化产物。没有碎片离子的化合物从源内CID碎片或在完整的单质谱中无法区分的异构体中分离出的碎片（或具有低强度/相对丰度的碎片），开发了“靶向MS/MS”方法。此后，可以在QTOF-MS/MS模式中使用碰撞能（CE）进一步分析这些化合物。研究了线性和检测限。在大多数情况下，废水和沃茨中的MDLs分别低于或等于5和2 ng/L，只有15种化合物的MDLs在5和50 ng/L之间。该方法已应用于真实的样品，所得结果表明，大部分的废水中的L浓度在两个数量级以上呈线性关系。所创建的数据库中包含的药物活性化合物以ng/L和μ g/L范围内的浓度存在于水样中。L水平，并且在数据库中包含的300种农药中的大多数样品中也检测到2至15种农药。除了数据库中包含的化合物之外，还发现了一些降解产物，从而揭示了该方法作为分析农药的有用工具。沃茨中的有机微污染物（C）2010 Elsevier B V版权所有
In this study we have developed and evaluated an analytical method for a rapid automated screening and confirmation of a large number of organic micro-contaminants (almost 400) and also the quantification of the positive findings in water samples of different types (surface and wastewaters) using liquid chromatography-electrospray quadrupole-time-of-flight mass spectrometry (LC-QTOFMS) based on the use of an accurate-mass database The created database includes data not only on the accurate masses of the target ions but also on the characteristic in-source fragment ions isotopic pattern and retention time data This customized database was linked to commercially available software which extracted all the potential compounds of interest from the LC-QTOFMS raw data of each sample and matched them against the database to search for targeted compounds in the sample The detailed fragmentation information has also been used as a powerful tool for the automatic identification of unknown compounds and/or transformation products with similar structures to those of known organic contaminants included in the database The database can be continually enlarged To confirm identification of compounds which have no fragment ions (or fragments with low intensity/relative abundance) from in-source CID fragmentation or isomers which are not distinguished within full single mass spectra a "Targeted MS/MS" method is developed Thereafter these compounds can be further analyzed using the collision energy (CE) in QTOF-MS/MS mode Linearity and limits of detection were studied Method detection limits (MDLs) in effluent wastewater and river waters were in most cases lowers or equal to 5 and 2 ng/L respectively Only 15 compounds had MDLs between 5 and 50 ng/L in effluent wastewater matrix We obtained a linearity of the calibration curves over two orders of magnitude The method has been applied to real samples and the results obtained reveal that most of the pharmaceutically active compounds contained in the created database were present in the water samples with concentrations in the range of ng/L and mu g/L levels and in most of the samples between 2 and 15 pesticides of the 300 contained in the database were also detected In addition to the compounds included in the database some degradation products were found thus revealing the method as a useful tool for the analysis of organic micro-contaminants in waters (C) 2010 Elsevier B V All rights reserved