Fedtke N, Bolt H M
Int Arch Occup Environ Health. 1986;57(2):149-58. doi: 10.1007/BF00381383.
Male Wistar rats were exposed to 1000 ppm n-hexane, and the excreted urinary metabolites were analyzed by capillary gas chromatography-mass spectrometry (GC-MS). 1-Hexanol, 2-hexanol, 3-hexanol, 2-hexanone, 2,5-hexanedione, 2,5-dimethyltetrahydrofuran, 2,5-dimethyl-2,3-dihydrofuran and gamma-valerolactone were identified by their retention times and their mass spectra. Quantitative gas chromatographic analyses were performed using an FID. Experiments on the hydrolysis of conjugated n-hexane metabolites revealed that enzymatic hydrolysis (in addition to acid hydrolysis) was not required, as treatment with HCl hydrolyzed conjugates sensitive to acid as well as conjugates sensitive to beta-glucuronidase. By incorporating acid hydrolysis only and by using C18-cartridges for sample extraction, a method was developed that allowed the determination of n-hexane metabolites with a sample preparation time of only 45 min. Assay precision was assessed by repeated analyses of the same urine sample. Coefficients of variation for the individual metabolites ranged from between 1.8 and 3.3.
将雄性Wistar大鼠暴露于1000 ppm的正己烷中，并用毛细管气相色谱 - 质谱联用仪（GC-MS）分析其排泄的尿液代谢产物。通过保留时间和质谱鉴定出1-己醇、2-己醇、3-己醇、2-己酮、2,5-己二酮、2,5-二甲基四氢呋喃、2,5-二甲基-2,3-二氢呋喃和γ-戊内酯。使用氢火焰离子化检测器（FID）进行定量气相色谱分析。对共轭正己烷代谢产物的水解实验表明，不需要酶水解（除了酸水解），因为用盐酸处理可水解对酸敏感的共轭物以及对β-葡萄糖醛酸酶敏感的共轭物。通过仅采用酸水解并使用C18柱进行样品萃取，开发了一种方法，该方法仅需45分钟的样品制备时间即可测定正己烷代谢产物。通过对同一份尿液样品进行重复分析来评估测定精密度。各个代谢产物的变异系数在1.8至3.3之间。
