Allsup T, Walsh D
J Chromatogr. 1982 Feb 19;236(2):421-8. doi: 10.1016/s0021-9673(00)84892-x.
An analytical method for phenols has been adapted for the analysis of chlorophenylmercapturic acids in rat urine. Chlorothiophenols were produced from the mercapturic acids by hydrolytic cleavage with sodium hydroxide. Acetate esters of the chlorothiophenols were formed by addition of acetic anhydride to the aqueous alkaline solution. After acylation, the acetate derivatives were extracted into hexane. Forming the acetate esters of the chlorothiophenols prevented their oxidation to disulfides and significantly improved their chromatographic properties. Electron-capture gas chromatographic analysis of the stable acetate esters was performed on a mixed phase column, 4% SE-30 + 6% OV-210. Recoveries of four chlorothiophenols ranged from 82 to 93%. This method required no sample transfer steps; therefore, sample loss and analysis time were minimized.
一种用于酚类分析的方法已被改编用于分析大鼠尿液中的氯苯巯基尿酸。氯硫酚由巯基尿酸通过用氢氧化钠进行水解裂解制得。氯硫酚的乙酸酯通过向碱性水溶液中加入乙酸酐形成。酰化后，乙酸酯衍生物被萃取到己烷中。形成氯硫酚的乙酸酯可防止它们氧化为二硫化物，并显著改善其色谱性质。在混合相柱（4% SE - 30 + 6% OV - 210）上对稳定的乙酸酯进行电子捕获气相色谱分析。四种氯硫酚的回收率在82%至93%之间。该方法无需样品转移步骤；因此，样品损失和分析时间被降至最低。
