Analysis of triclocarban in aquatic samples by liquid chromatography electrospray ionization mass spectrometry
Analysis of triclocarban in aquatic samples by liquid chromatography electrospray ionization mass spectrometry
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DOI：
10.1021/es049524f
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发表时间：
2004-09-15
影响因子：
11.4
通讯作者：
Paull, DH
中科院分区：
文献类型：
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作者：
Halden, RU;Paull, DH
三氯卡班，N-(4-chlorophenyl)-N‘-(3，4-dichlorophenyl)urea，是一种多氯苯基脲杀虫剂，以Tcc商标上市，主要用作个人护理产品的抗菌添加剂。尽管几十年来它被广泛使用，但关于TCC的环境发生数据很少。这在一定程度上是由于缺乏提供所需的灵敏度、选择性、可负担性和易用性的分析技术。为了满足这一需求，本文介绍了一种能够在ng/L水平上测定水环境中TCC浓度的高效电喷雾电离质谱仪(LC/ESI/MS)。TCC通过固相萃取从水样中浓缩，通过等度或梯度洗脱从C-18柱上分离干扰，并在负ESI模式下通过选择性监测作为参考离子的(M-H)(-)基峰(m/z 313)及其含氯-37的同位素(MLZ 315,317)进行检测和鉴定。分别提取和分析了水样中的颗粒物。以TCC和三氯生的稳定同位素为内标，实现了准确的定量。在流动相中加入10 mM的冰醋酸可生成([M-H+60](-))加合物，该加合物被成功地用于提高方法的灵敏度和选择性，特别是在分析具有挑战性的环境基质时。方法检出限依赖于基质，范围为3~50 ng/L。在大巴尔的摩地区采集的36份样品中，河水和废水中的TCC浓度分别高达5600和6750 ng/L。原水和成品饮用水不含可检测到的杀虫剂(
Triclocarban, N-(4-chlorophenyl)-N'-(3,4-dichlorophenyl)urea, is a polychlorinated phenyl urea pesticide, marketed under the trademark TCC and used primarily as an antibacterial additive in personal care products. Despite its extensive use over several decades, environmental occurrence data on TCC are scarce. This is due in part to a lack of analytical techniques offering the desired sensitivity, selectivity, affordability, and ease of use. This need is addressed here by introducing a liquid chromatography electrospray ionization mass spectrometry (LC/ESI/MS) method allowing for the determination of TCC concentrations in aquatic environments at the ng/L level. TCC was concentrated from aqueous samples by solid-phase extraction, separated from interferences on a C-18 column by either isocratic or gradient elution, and detected and identified in negative ESI mode by selectively monitoring the (M - H)(-) base peak (m/z 313) and its Cl-37-containing isotopes (mlz 315, 317) that served as reference ions. Particulates contained in aquatic samples were extracted and analyzed separately. Accurate quantification was achieved using stable isotopes of TCC and triclosan as internal standards. Addition of 10 mM acetic acid to the mobile phase yielded acetic acid adducts ([M - H + 60](-)) that were successfully exploited to boost method sensitivity and selectivity, especially when analyzing challenging environmental matrixes. Method detection limits were matrix dependent, ranging from 3 to 50 ng/L. In 36 grab samples obtained from the Greater Baltimore area, TCC was detected in river water and wastewater at concentrations of up to 5600 and 6750 ng/L, respectively. Raw and finished drinking water did not contain detectable quantities of the pesticide (