Wadsworth Center, New York State Department of Health, and Department of Environmental Health Sciences, School of Public Health, State University of New York at Albany, Albany, NY, USA; Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimioupolis Zografou, Athens, Greece.
Wadsworth Center, New York State Department of Health, and Department of Environmental Health Sciences, School of Public Health, State University of New York at Albany, Albany, NY, USA.
J Chromatogr A. 2014 Jan 10;1324:141-8. doi: 10.1016/j.chroma.2013.11.031. Epub 2013 Nov 21.
A liquid-liquid extraction (LLE; ethyl acetate) protocol, followed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) methodology, was developed for the determination of 19 compounds, including bisphenol A diglycidyl ethers (BADGEs; industrial ethers), benzophenone-type UV filters (BP-UV filters; precursors and metabolites), p-hydroxybenzoic acid esters (parabens; preservatives), triclosan (TCS) and triclocarban (TCC) in human urine. Urine specimens were enzymatically deconjugated with β-glucuronidase (from Helix pomatia) and extracted by a LLE procedure for the measurement of total concentrations (i.e., free+conjugated forms) of target analytes. Absolute recoveries of BADGEs, BP-UV filters, parabens, TCS and TCC ranged 25-135%, 84-125%, 52-126%, 75-118% and 90-124%, respectively. Method precision (absolute values; N=5 replicate analyses at the fortification level of 10 ng, k=5 days) ranged from 5.8 (ethyl paraben) to 24.0% (TCS). The limits of quantification (LOQs) varied depending on the target compound and generally ranged from 0.2 to 2.0 ng/mL. The matrix effects ranged from +11 (2,3,4-trihydroxybenzophenone) to -86% (2,4-dihydroxybenzophenone). A total of 30 urine specimens collected from Athens, Greece, were analyzed for the 19 target compounds to demonstrate the applicability of the developed method. The concentrations of target chemicals in urine were presented on volume-, specific gravity (SG)-, and creatinine-normalization bases. MeP, EtP, PrP, OH-EtP, BADGE·2H2O, BP-1 and TCS were found frequently in urine at concentrations in the range of 2.7-436 ng/mL, <0.5-25.4 ng/mL, <0.5-575 ng/mL, <2-18.4 ng/mL, <0.5-13.8 ng/mL, <1-14.6 ng/mL and <0.5-95.3 ng/mL, respectively.
建立了一种液-液萃取（LLE；乙酸乙酯）方法，结合液相色谱-电喷雾串联质谱法（LC-ESI-MS/MS），用于测定 19 种化合物，包括双酚 A 二缩水甘油醚（BADGEs；工业醚）、二苯甲酮型紫外线滤光剂（BP-UV 滤光剂；前体和代谢物）、对羟基苯甲酸酯（对羟基苯甲酸酯；防腐剂）、三氯生（TCS）和三氯卡班（TCC）在人尿中的含量。尿液样本用β-葡糖苷酸酶（来自大蜗牛）进行酶解共轭，然后通过 LLE 程序提取，以测量目标分析物的总浓度（即游离+共轭形式）。BADGEs、BP-UV 滤光剂、对羟基苯甲酸酯、TCS 和 TCC 的绝对回收率分别为 25-135%、84-125%、52-126%、75-118%和 90-124%。方法精密度（绝对值；N=5 次重复分析，浓度为 10 ng，k=5 天）为 5.8%（乙基对羟基苯甲酸酯）至 24.0%（TCS）。定量限（LOQ）因目标化合物而异，通常为 0.2-2.0ng/mL。基质效应范围为+11（2,3,4-三羟基二苯甲酮）至-86%（2,4-二羟基二苯甲酮）。从希腊雅典采集了 30 份尿液样本，用于分析 19 种目标化合物，以证明所开发方法的适用性。目标化学物质在尿液中的浓度分别以体积、比重（SG）和肌酐归一化基础表示。MeP、EtP、PrP、OH-EtP、BADGE·2H2O、BP-1 和 TCS 经常在尿液中以 2.7-436ng/mL、<0.5-25.4ng/mL、<0.5-575ng/mL、<2-18.4ng/mL、<0.5-13.8ng/mL、<1-14.6ng/mL 和<0.5-95.3ng/mL 的浓度范围内存在。
