Kataoka H, Manabe K, Nakase S, Makita M
Faculty of Pharmaceutical Sciences, Okayama University, Japan.
J Pharm Biomed Anal. 1991;9(9):699-704. doi: 10.1016/0731-7085(91)80209-r.
A capillary gas chromatographic (GC) method for the simultaneous determination of urinary hippuric acid (HA) and o-, m- and p-methylhippuric acids (MHAs), metabolites of toluene and o-, m- and p-xylenes, respectively, is described. These metabolites are converted into their isopropyl derivatives by extractive alkylation with tetrahexylammonium ion as extracting agent and isopropyl bromide as alkylating reagent in benzene. The derivatives are analysed using a chromatograph equipped with hydrogen flame ionization detector, split injection system and DB-17 capillary column. Benzoylleucine is used as an internal standard. The derivatives are well separated within 5 min and no interfering peaks are observed. The calibration curves of HA and MHAs in the range 1-50 micrograms are linear and sufficiently reproducible for quantitative analysis. Urine can be analysed accurately and precisely by this method without prior clean-up of the sample.
本文描述了一种毛细管气相色谱（GC）法，用于同时测定尿中马尿酸（HA）以及邻、间、对甲基马尿酸（MHA），它们分别是甲苯和邻、间、对二甲苯的代谢产物。这些代谢产物通过用四己基铵离子作为萃取剂、异丙基溴作为烷基化试剂在苯中进行萃取烷基化反应，转化为它们的异丙基衍生物。使用配备氢火焰离子化检测器、分流进样系统和DB - 17毛细管柱的色谱仪对衍生物进行分析。苯甲酰亮氨酸用作内标。衍生物在5分钟内得到良好分离，未观察到干扰峰。HA和MHA在1 - 50微克范围内的校准曲线呈线性，且对于定量分析具有足够的重现性。该方法无需对样品进行预先净化即可准确、精确地分析尿液。
