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开发固相萃取液相色谱串联质谱法测定废水中和回用水中的苯并三唑和苯并噻唑。

Development of a solid-phase extraction liquid chromatography tandem mass spectrometry method for benzotriazoles and benzothiazoles in wastewater and recycled water.

机构信息

Curtin Water Quality Research Centre, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845, Australia.

出版信息

J Chromatogr A. 2013 Jul 19;1299:48-57. doi: 10.1016/j.chroma.2013.04.073. Epub 2013 May 3.

DOI:10.1016/j.chroma.2013.04.073
PMID:23768537
Abstract

Two methods employing solid-phase extraction and liquid chromatography tandem mass spectrometry were developed for the analysis of benzotriazoles (BTs) and benzothiazoles (BThs), compounds which are commonly found in a large variety of commercial and household products. The first method was able to detect 7 BTs and 7 BThs, the largest suite of BTs and BThs analysed in a single method to-date, but could not distinguish between the isomers, 4-methylbenzotriazole (4-MeBT) and 5-methylbenzotriazole (5-MeBT). Therefore, a second method was developed to achieve the chromatographic separation of 4-MeBT and 5-MeBT. The methods were validated for ultrapure water and secondary wastewater, and method limits of detection (MLD) for BTs and BThs (for the primary method) ranged from 0.1 to 58ngL(-1) for ultrapure water, and 2 to 322ngL(-1) for secondary wastewater. For the secondary method, MLDs for 4- and 5-MeBT ranged from 8 to 12ngL(-1) for ultrapure water, and 388 to 406ngL(-1) for secondary wastewater. Analysis of secondary wastewater and reverse osmosis (RO) treated water from an advanced water recycling plant in Australia is presented, and represents the first reported data from the analysis of BTs and BThs in recycled water. Some of these compounds were found to persist through wastewater treatment and incompletely removed by RO treatment. Benzotriazole (BT), 4-MeBT, 5-MeBT and 2-(methylthio)benzothiazole were detected in secondary wastewater, however the latter compound was not quantifiable. Concentrations of BT and tolyltriazoles (TTs, i.e. sum of 4- and 5-MeBT, detected with the primary method) in secondary wastewater were 3.3 (±0.02) and 2.8 (±0.04)μgL(-1), respectively. These same compounds were also detected in the post-RO water samples at concentrations of 974 (±28)ngL(-1) for BT and 416(±34)ngL(-1) for TTs. 2-Hydroxybenzothiazole was also detected in the post-RO water samples, however it was not quantifiable. Removal efficiencies for RO treatment were calculated to be between 70% and 85% for BT and TTs.

摘要

两种方法采用固相萃取和液相色谱串联质谱法,用于分析苯并三唑(BTs)和苯并噻唑(BThs),这些化合物通常存在于各种商业和家用产品中。第一种方法能够检测到 7 种 BTs 和 7 种 BThs,是迄今为止在单一方法中分析的最大的 BTs 和 BThs 套件,但无法区分异构体 4-甲基苯并三唑(4-MeBT)和 5-甲基苯并三唑(5-MeBT)。因此,开发了第二种方法来实现 4-MeBT 和 5-MeBT 的色谱分离。该方法对超纯水和二级废水进行了验证,BTs 和 BThs 的方法检出限(MLD)(对于主要方法)范围为超纯水的 0.1 至 58ngL(-1),二级废水的 2 至 322ngL(-1)。对于第二种方法,4-和 5-MeBT 的 MLD 范围为超纯水的 8 至 12ngL(-1),二级废水的 388 至 406ngL(-1)。对澳大利亚高级水回收厂的二级废水和反渗透(RO)处理水进行了分析,这是首次报道从再生水中分析 BTs 和 BThs 的数据。这些化合物中的一些在废水处理过程中被发现仍然存在,并且 RO 处理不能完全去除。二级废水中检测到苯并三唑(BT)、4-MeBT、5-MeBT 和 2-(甲硫基)苯并噻唑,但后一种化合物无法定量。二级废水中 BT 和甲苯三唑(TTs,即检测到的 4-和 5-MeBT 之和)的浓度分别为 3.3(±0.02)和 2.8(±0.04)μgL(-1)。在 RO 处理后的水样中也检测到这些相同的化合物,BT 的浓度为 974(±28)ngL(-1),TTs 的浓度为 416(±34)ngL(-1)。在 RO 处理后的水样中还检测到 2-羟基苯并噻唑,但无法定量。RO 处理的去除效率计算为 BT 和 TTs 的 70%至 85%。

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