Wadsworth Center, New York State Department of Health, School of Public Health, State University of New York at Albany, United States.
Anal Chem. 2013 Jan 2;85(1):441-8. doi: 10.1021/ac303266m. Epub 2012 Dec 17.
Benzotriazole (BTR) and benzothiazole (BTH) derivatives are used in a wide variety of industrial and consumer products and have been reported to occur in the environment. Owing to a lack of analytical methods, human exposure to BTR and BTH is still unknown. In this study, a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI(+)MS/MS) method was developed for simultaneous determination of five 1,2,3-benzotriazoles and five 1,3-benzothiazoles in human urine. The target benzotriazoles were 1H-benzotriazole, 1-hydroxy-benzotriazole, tolyltriazole, xylyltriazole (or 5,6-dimethyl-1H-benzotriazole), and 5-chloro-benzotriazole, and the target benzothiazoles were benzothiazole, 2-hydroxy-benzothiazole, 2-methylthio-benzothiazole, 2-amino-benzothiazole, and 2-thiocyanomethylthio-benzothiazole. Urine specimens were enzymatically deconjugated with β-glucuronidase and extracted by a solid-phase extraction (SPE) procedure for the measurement of total concentrations (i.e., free + conjugated forms) of BTRs and BTHs. Additionally, a liquid-liquid extraction (LLE) method was developed for comparison of extraction efficiencies between SPE and LLE. The limits of detection (LODs) ranged from 0.07 (2-amino-benzothiazole) to 4.0 ng/mL (benzothiazole) for the SPE method and from 0.04 (tolyltriazole) to 6.4 ng/mL (benzothiazole) for the LLE method. A total of 100 urine specimens, collected from Athens, Greece, were analyzed by enzymatic deconjugation and SPE. Benzothiazole and tolyltriazole were found frequently, and their concentrations were on the order of a few ng/mL. To our knowledge, this is the first study on the occurrence of 10 BTR and BTH compounds in human urine.
苯并三唑（BTR）和苯并噻唑（BTH）衍生物广泛应用于各种工业和消费产品中，并且已被报道存在于环境中。由于缺乏分析方法，人类接触 BTR 和 BTH 的情况仍不清楚。在这项研究中，开发了一种液相色谱-电喷雾电离串联质谱（LC-ESI(+)MS/MS）方法，用于同时测定人尿中五种 1,2,3-苯并三唑和五种 1,3-苯并噻唑。目标苯并三唑为 1H-苯并三唑、1-羟基苯并三唑、甲苯三唑、二甲苯三唑（或 5,6-二甲基-1H-苯并三唑）和 5-氯苯并三唑，目标苯并噻唑为苯并噻唑、2-羟基苯并噻唑、2-甲基硫代苯并噻唑、2-氨基苯并噻唑和 2-硫氰基甲基硫代苯并噻唑。尿样用β-葡糖苷酸酶酶解后，通过固相萃取（SPE）程序提取，用于测定 BTRs 和 BTHs 的总浓度（即游离+共轭形式）。此外，还开发了液-液萃取（LLE）方法，比较 SPE 和 LLE 之间的萃取效率。SPE 方法的检出限（LOD）范围为 0.07（2-氨基苯并噻唑）至 4.0 ng/mL（苯并噻唑），LLE 方法的 LOD 范围为 0.04（甲苯三唑）至 6.4 ng/mL（苯并噻唑）。从希腊雅典采集了 100 份尿样，通过酶解和 SPE 进行分析。苯并噻唑和甲苯三唑频繁出现，其浓度为数 ng/mL。据我们所知，这是首次研究 10 种 BTR 和 BTH 化合物在人尿中的存在情况。
