Simultaneous determination of triclocarban and triclosan in municipal biosolids by liquid chromatography tandem mass spectrometry

Simultaneous determination of triclocarban and triclosan in municipal biosolids by liquid chromatography tandem mass spectrometry
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DOI:
10.1016/j.chroma.2007.07.024
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发表时间:
2007-09-14
影响因子:
4.1
通讯作者:
Metcalfe, Cms D.
Metcalfe, Cms D.
中科院分区:
化学2区
文献类型:
--
作者:
Chu, Shaogang;Metcalfe, Cms D.

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开发了一种灵敏而准确的方法,用于同时测定城市污水处理厂 (WWTP) 污泥和处理过的生物固体中的三氯生和三氯卡班。这些方法包括通过加压液体萃取 (PLE) 进行萃取,然后在 Oasis HLB 固相萃取 (SPE) 柱上净化样品,并通过液相色谱、电喷雾电离和串联质谱 (LC-ESI-MS/MS) 进行分析。使用三氯生和三氯卡班的稳定同位素作为内标,通过同位素稀释实现准确定量。通过标准添加法评估加标生物固体样品 (n = 5) 中的基质效应 (ME),这些分析表明三氯生和三氯卡班的平均 ME 值分别为 79.7 +/- 6.7 和 100.5 +/- 8.4%;表明该样品净化方法有效去除了干扰。加标生物固体样品中三氯生和三氯卡班的平均回收率分别为 97.7 +/- 6.2 和 98.3 +/- 5,三氯生和三氯卡班的检测限 (LOD) 分别为 1.5 和 0.2 ng/g (d.w.)。该方法适用于分析从加拿大安大略省三个污水处理厂收集的活性污泥和处理过的生物固体样品中的三氯生和三氯卡班。这些初步结果表明,三氯生和三氯卡班共存于城市污泥和处理过的生物固体中,三氯生浓度范围为 0.62 至 11.55 微克/克干重,三氯卡班浓度范围为 2.17 至 5.97 微克/克干重。 (c) 2007 年 Elsevier B.V. 出版
A sensitive and accurate method was developed for the simultaneous determination of triclosan and triclocarban in sludge and treated biosolids from municipal wastewater treatment plants (WWTPs). The methods involved extraction by pressurized liquid extraction (PLE), followed by sample clean-up on a Oasis HLB solid phase extraction (SPE) cartridge and analysis by liquid chromatography with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS). Accurate quantification was achieved by isotope dilution using stable isotopes of triclosan and triclocarban as internal standards. Matrix effects (ME) in samples of spiked biosolids (n = 5) were evaluated by a standard addition method, and these analyses indicated mean ME values of 79.7 +/- 6.7 and 100.5 +/- 8.4% for triclosan and triclocarban, respectively; indicating that the sample clean-up method effectively removed interferences. The mean recoveries from the spiked biosolids sample were 97.7 +/- 6.2 and 98.3 +/- 5 for triclosan and triclocarban, respectively, and the limits of detection (LOD) were 1.5 and 0.2 ng/g (d.w.) for triclosan and triclocarban, respectively. The method was applied to the analysis of triclosan and triclocarban in samples of activated sludge and treated biosolids collected from three WWTPs in Ontario, Canada. These preliminary results indicate that triclosan and triclocarban co-occur in municipal sludge and treated biosolids at concentrations ranging from 0.62 to 11.55 mu g/g dry weight for triclosan, and from 2.17 to 5.97 mu g/g dry weight for triclocarban. (c) 2007 Published by Elsevier B.V.