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搅拌棒吸附萃取-液相解吸-液相色谱-串联质谱法定量测定废水中三氯卡班。

Quantitative determination of triclocarban in wastewater effluent by stir bar sorptive extraction and liquid desorption-liquid chromatography-tandem mass spectrometry.

机构信息

Department of Chemistry, The College of Wooster, 943 College Mall, Wooster, OH 44691, USA.

出版信息

J Chromatogr A. 2010 Mar 12;1217(11):1742-7. doi: 10.1016/j.chroma.2010.01.028. Epub 2010 Jan 18.

Abstract

Triclocarban is an antimicrobial and antibacterial agent found in personal care products and subsequently is a prevalent wastewater contaminant. A quantitative method was developed for the analysis of triclocarban in wastewater effluents using stir bar sorptive extraction-liquid desorption (SBSE-LD) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) by means of an electrospray interface. A stir bar coated with polydimethylsiloxane (PDMS) is placed within a vial containing wastewater effluent and is stirred for an hour at room temperature. The PDMS stir bar is then placed in a LC vial containing methanol and is desorbed in a sonicator bath. The methanol is evaporated to dryness and reconstituted in 75% methanol. Spike and recovery experiments in groundwater that did not contain native concentrations of triclocarban were performed at 0.5 microg/L and were 93+/-8%. Recoveries in wastewater effluent that were corrected for the background levels of triclocarban were 92+/-2% and 96+/-5%, respectively, when spiked with 0.5 and 5 microg/L of triclocarban. The precision of the method as indicated by the relative standard error was 2%. The limit of quantitation was 10 ng/L. The SBSE-LD-LC/MS/MS method was applied to wastewater effluent samples collected from northeast Ohio. Triclocarban was quantitated in all five effluent samples, and its concentration ranged from 50 to 330 ng/L. The described method demonstrates a simple, green, low-sample volume, yet, sensitive method to measure triclocarban in aqueous matrices.

摘要

三氯卡班是一种存在于个人护理产品中的抗菌和抑菌剂,因此也是一种普遍存在的废水中污染物。本研究采用搅拌棒吸附萃取-液解吸(SBSE-LD)与液相色谱-串联质谱(LC-MS/MS)联用技术,建立了一种测定废水中三氯卡班的定量方法。该方法采用带有聚二甲基硅氧烷(PDMS)涂层的搅拌棒,将其置于含有废水的小瓶中,在室温下搅拌 1 小时。然后,将 PDMS 搅拌棒置于含有甲醇的 LC 小瓶中,在超声浴中进行解吸。将甲醇蒸发至干燥,然后在 75%甲醇中重新配制。在未含有天然浓度三氯卡班的地下水样品中进行了 0.5μg/L 的加标和回收实验,回收率为 93+/-8%。经背景水平三氯卡班校正后,在废水样品中加标 0.5 和 5μg/L 的三氯卡班,回收率分别为 92+/-2%和 96+/-5%。该方法的精密度(相对标准误差)为 2%。定量限为 10ng/L。该 SBSE-LD-LC/MS/MS 方法应用于从俄亥俄州东北部采集的废水样品。在所有五个废水样品中都定量了三氯卡班,其浓度范围为 50-330ng/L。该方法简单、绿色、低样品量、灵敏,可用于测定水基质中的三氯卡班。

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