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高效液相色谱法同时测定人体组织中的百草枯和敌草快

Simultaneous determination of paraquat and diquat in human tissues by high-performance liquid chromatography.

作者信息

Ito S, Nagata T, Kudo K, Kimura K, Imamura T

机构信息

Department of Forensic Medicine, Faculty of Medicine, Kyushu University, Fukuoka, Japan.

出版信息

J Chromatogr. 1993 Jul 23;617(1):119-23. doi: 10.1016/0378-4347(93)80429-8.

Abstract

A simple, sensitive, reliable, and economical method for simultaneous determination of paraquat dichloride and diquat dibromide in human biological materials has been developed, using high-performance liquid chromatography. The drugs were extracted from the sample with a Sep-Pak C18 cartridge and applied to a chromatograph with the internal standard, L-tyrosine. Paraquat and diquat were clearly separated on the octadecylsilica column with a mobile phase of 0.5% potassium bromide in 5% methanol solution, containing triethylamine (1 ml/l). The pH of the mobile phase was adjusted to 3-4 with 1.3 M phosphoric acid. Two ultraviolet wavelengths were selected, 256 nm for paraquat as well as the internal standard, and 310 nm for diquat. The calibration curves were linear in the concentration range 0.1-10 micrograms/g, and the lower limit of detection was 0.05 microgram/g. We used this method to examine the concentrations of paraquat and diquat in tissues of an individual at autopsy.

摘要

已开发出一种使用高效液相色谱法同时测定人体生物材料中百草枯二氯化物和敌草快二溴化物的简单、灵敏、可靠且经济的方法。药物用Sep-Pak C18柱从样品中萃取出来,并与内标L-酪氨酸一起应用于色谱仪。百草枯和敌草快在十八烷基硅胶柱上能被清晰分离,流动相为含三乙胺(1毫升/升)的5%甲醇溶液中的0.5%溴化钾。用1.3M磷酸将流动相的pH值调节至3 - 4。选择了两个紫外波长,百草枯及其内标为256nm,敌草快为310nm。校准曲线在0.1 - 10微克/克的浓度范围内呈线性,检测下限为0.05微克/克。我们使用该方法检测了一名个体尸检组织中百草枯和敌草快的浓度。

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