Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, GA 30341, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jan 15;881-882:27-33. doi: 10.1016/j.jchromb.2011.11.024. Epub 2011 Nov 26.
3,4,4'-Trichlorocarbanilide (triclocarban, TCC) is widely used as an antimicrobial agent in a variety of consumer and personal care products. Because of its widespread use, the potential for human exposure to TCC is high. Human exposure to TCC may be assessed by measuring the concentrations of conjugated or free species of TCC and its two oxidative metabolites, 2'-hydroxy-TCC (2'-OH-TCC) and 3'-hydroxy-TCC (3'-OH-TCC), in urine or serum. To assess human exposure to TCC, we developed a method that uses restricted access materials (RAM) on-line solid phase extraction (SPE) coupled to high performance liquid chromatography-isotope dilution tandem mass spectrometry with peak focusing (HPLC-MS/MS). Sample clean-up by RAM relies on both size exclusion chromatography, to remove the high-molecular matrix components, and reversed phase partition, to extract and pre-concentrate the target analytes. TCC, 2'-OH-TCC and 3'-OH-TCC present in urine or serum were concentrated on the RAM SPE column, back-eluted from the SPE column, diluted through a mixing tee for peak focusing, separated by HPLC, and detected by isotope dilution-MS/MS. The method required a small amount of sample (50 μL) and minimal sample pretreatment. The limits of detection (LOD) ranged from 0.01 to 0.1 ng/mL. The method was applied to measure TCC and its metabolites in 158 urine and 16 serum samples collected from adults with no known exposure to TCC. TCC was detected in 35.4% of the urine samples (range: <LOD to 401 ng/mL). This sensitive method is rugged as well as labor- and cost-effective, and allows for the analysis of a large number of samples for epidemiological studies.
3,4,4'-三氯卡班（三氯生，TCC）作为一种抗菌剂广泛应用于各种消费品和个人护理产品中。由于其广泛使用，人类接触 TCC 的潜在风险很高。可以通过测量尿液或血清中 TCC 及其两种氧化代谢物 2'-羟基-TCC（2'-OH-TCC）和 3'-羟基-TCC（3'-OH-TCC）的共轭或游离浓度来评估人体对 TCC 的暴露情况。为了评估人体对 TCC 的暴露情况，我们开发了一种使用受限访问材料（RAM）在线固相萃取（SPE）结合高效液相色谱-同位素稀释串联质谱法与峰聚焦（HPLC-MS/MS）的方法。通过 RAM 进行样品净化，同时采用尺寸排阻色谱法去除高分子基质成分，采用反相分配法提取和预浓缩目标分析物。尿液或血清中的 TCC、2'-OH-TCC 和 3'-OH-TCC 被浓缩在 RAM SPE 柱上，从 SPE 柱上洗脱下来，通过混合三通进行稀释以实现峰聚焦，通过 HPLC 进行分离，并通过同位素稀释-MS/MS 进行检测。该方法需要少量样品（50μL），且样品预处理量很少。检测限（LOD）范围为 0.01 至 0.1ng/mL。该方法应用于测量 158 份尿液和 16 份血清样本中的 TCC 及其代谢物，这些样本均来自未接触过 TCC 的成年人。在 35.4%的尿液样本中检测到 TCC（范围：<LOD 至 401ng/mL）。这种灵敏的方法具有坚固耐用、节省劳力和成本效益高的特点，可用于对大量样本进行流行病学研究。
