采用超高效液相色谱/电喷雾串联质谱法同时测定尿液和血清中的三氯生、三氯卡班、三氯卡班代谢物和副产物。
Simultaneous determination of triclosan, triclocarban, triclocarban metabolites and byproducts in urine and serum by ultra-high-performance liquid chromatography/electrospray ionization tandem mass spectrometry.
机构信息
State Key Laboratory of Environmental and Biological Analysis, Department of Chemistry, Hong Kong Baptist University, Hong Kong, 999077, China.
HKBU Institute for Research and Continuing Education, Shenzhen, Guangdong, 518000, China.
出版信息
Rapid Commun Mass Spectrom. 2021 Jul 31;35(14):e9117. doi: 10.1002/rcm.9117.
RATIONALE
Triclosan (TCS) and triclocarban (TCC) are ubiquitous antimicrobial agents incorporated in consumer and personal care products. Due to their human health risks, it is essential to develop a sensitive and accurate analytical method to simultaneously quantify TCS, TCC, as well as their metabolites and byproducts in urine and serum samples.
METHODS
The quantitative parameters of TCS, TCC, TCC metabolites and byproducts (2'-OH-TCC, 3'-OH-TCC, 6-OH-TCC, DHC, DCC, NCC) were optimized by using ultra-high-performance liquid chromatography/electrospray ionization tandem mass spectrometry (UHPLC/ESI-MS/MS). Enzymatic hydrolysis of the samples was optimized based on enzyme dosage and incubation time. The efficiencies of solid-phase extraction (SPE) and liquid-liquid extraction (LLE) were compared. The effectiveness of the established method was evaluated, and method application was validated using real urine and serum samples.
RESULTS
The conjugates were sufficiently hydrolyzed under 500 U/mL β-glucuronidase and 80 U/mL sulfatase at 37°C for 4 h. Compared with the LLE method, SPE achieved higher extraction efficiency in both urine and serum samples. The optimized SPE-UHPLC/ESI-MS/MS method showed low limits of detection (LODs) in the range 0.001-0.3 ng/mL and good linearity (R > 0.99) at 0.01-150 ng/mL in both matrices. Excellent recoveries of 82.0%-120.7% (urine) and 76.7%-113.9% (serum) were obtained with low relative standard deviation (RSD, <7.6%) for inter-day and intra-day injections. This method was applicable to quantify target compounds in multiple biological urine and serum samples. Notably, TCS and TCC were detected with average concentrations of 8.37 and 10.46 ng/mL, respectively, in 15 Chinese female urine samples, with the simultaneous detection of TCC metabolites and byproducts.
CONCLUSIONS
A reliable method was established to simultaneously determine TCS, TCC, TCC metabolites and byproducts in urine and serum samples by using UHPLC/ESI-MS/MS. This sensitive methodology provides the basis for the evaluation of TCS and TCC exposure at the metabolic level.
背景
三氯生（TCS）和三氯卡班（TCC）是广泛应用于消费和个人护理产品中的抗菌剂。由于其对人类健康的潜在风险，开发一种灵敏、准确的分析方法来同时定量检测尿液和血清样本中的 TCS、TCC 及其代谢物和副产物至关重要。
方法
采用超高效液相色谱/电喷雾串联质谱法（UHPLC/ESI-MS/MS）对 TCS、TCC、TCC 代谢物和副产物（2'-OH-TCC、3'-OH-TCC、6-OH-TCC、DHC、DCC、NCC）的定量参数进行优化。基于酶剂量和孵育时间优化了样品的酶解条件。比较了固相萃取（SPE）和液液萃取（LLE）的效率。评估了所建立方法的有效性，并使用实际的尿液和血清样本验证了方法的适用性。
结果
在 37°C 下，500 U/mLβ-葡萄糖醛酸酶和 80 U/mL 磺基转移酶可充分水解结合物。与 LLE 方法相比，SPE 在尿液和血清样本中均具有更高的提取效率。优化的 SPE-UHPLC/ESI-MS/MS 方法在尿液和血清基质中的检测限（LOD）均为 0.001-0.3ng/mL，在 0.01-150ng/mL 范围内的线性良好（R>0.99）。尿液和血清中目标化合物的回收率均为 82.0%-120.7%（日内）和 76.7%-113.9%（日间），相对标准偏差（RSD，<7.6%）较低。该方法适用于定量分析多种生物尿液和血清样本中的目标化合物。值得注意的是，在 15 例中国女性尿液样本中，TCS 和 TCC 的平均浓度分别为 8.37 和 10.46ng/mL，同时检测到 TCC 代谢物和副产物。
结论
本研究建立了一种可靠的 UHPLC/ESI-MS/MS 方法，可同时定量检测尿液和血清样本中的 TCS、TCC、TCC 代谢物和副产物。该灵敏方法为评估 TCS 和 TCC 的代谢水平暴露提供了依据。
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