Kawaguchi Migaku, Ito Rie, Honda Hidehiro, Endo Naoyuki, Okanouchi Noriya, Saito Koichi, Seto Yasuo, Nakazawa Hiroyuki
Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, Hoshi University, 2-4-41 Ebara, Shinagawa-ku, Tokyo 142-8501, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Nov 15;875(2):577-80. doi: 10.1016/j.jchromb.2008.10.008. Epub 2008 Oct 14.
We have developed an analytical method for the determination of urinary 5-chloro-2-(2,4-dichlorophenoxy)phenol (triclosan), which utilizes stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS). Human urine sample is de-conjugated by treatment with beta-glucuronidase and sulfatase. A stir bar coated with polydimethylsiloxane (PDMS) is added to the urine sample in a vial and the sample is stirred for 60 min at room temperature (25 degrees C). Then, the PDMS stir bar is subjected to TD-GC-MS. The detection limit of triclosan is 0.05 ng mL(-1). The method shows linearity over the calibration range (0.1-10 ng mL(-1)) and the correlation coefficient (r) is higher than 0.993 for triclosan standard solution. The average recoveries of triclosan in human urine sample are 102.8-113.1% (RSD: 2.4-6.7%). This simple, sensitive, and selective analytical method may be used in the determination of trace amounts of triclosan in human urine samples.
我们开发了一种用于测定尿中5-氯-2-(2,4-二氯苯氧基)苯酚（三氯生）的分析方法，该方法采用搅拌棒吸附萃取（SBSE）和热脱附（TD）-气相色谱-质谱联用（GC-MS）技术。人体尿液样本经β-葡萄糖醛酸酶和硫酸酯酶处理后进行去结合反应。将一根涂有聚二甲基硅氧烷（PDMS）的搅拌棒加入到小瓶中的尿液样本中，在室温（25℃）下搅拌60分钟。然后，将PDMS搅拌棒进行热脱附-气相色谱-质谱分析。三氯生的检测限为0.05 ng mL⁻¹。该方法在校准范围（0.1 - 10 ng mL⁻¹）内呈线性，三氯生标准溶液的相关系数（r）高于0.993。人体尿液样本中三氯生的平均回收率为102.8 - 113.1%（相对标准偏差：2.4 - 6.7%）。这种简单、灵敏且具有选择性的分析方法可用于测定人体尿液样本中痕量的三氯生。
