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固相萃取后血浆和唾液中卡马西平及其10,11-环氧化物的高效液相色谱测定法

High-performance liquid chromatographic determination of carbamazepine and carbamazepine 10,11-epoxide in plasma and saliva following solid-phase sample extraction.

作者信息

Hartley R, Lucock M, Cookman J R, Becker M, Smith I J, Smithells R W, Forsythe W I

出版信息

J Chromatogr. 1986 Aug 2;380(2):347-56. doi: 10.1016/s0378-4347(00)83663-4.

DOI:10.1016/s0378-4347(00)83663-4
PMID:3760062
Abstract

A rapid, sensitive and simple to operate high-performance liquid chromatographic method for the simultaneous determination of carbamazepine (CBZ) and carbamazepine 10,11-epoxide (CBZ-EP) in plasma and saliva is described. The drug and its metabolite are extracted from both plasma and saliva using commercially available reversed-phase octadecylsilane bonded silica columns (Bond-Elut C18, 2.8 ml capacity). Separation of CBZ and CBZ-EP was achieved by reversed-phase chromatography, using a mobile phase consisting of acetonitrile-methanol-water (19:37:44) at a flow-rate of 1.8 ml/min in conjunction with a Nova-Pak C18 column. The analytical column, in Radial-Pak cartridge form, was used in combination with a Z-module RCSS and protected by a Guard-Pak precolumn module containing a Guard-Pak mu Bondapak C18 insert. Using ultraviolet detection at 214 nm, levels in the region of 50-100 ng/ml for CBZ and CBZ-EP can be measured with only 250 and 500 microliters of plasma and saliva, respectively. The method, which has been used to determine steady-state concentrations of the drug and its metabolite in paediatric patients receiving CBZ monotherapy, is also suitable for pharmacokinetic studies.

摘要

本文描述了一种快速、灵敏且操作简单的高效液相色谱法,用于同时测定血浆和唾液中的卡马西平(CBZ)及其10,11-环氧化物代谢物(CBZ-EP)。药物及其代谢物从血浆和唾液中提取,采用市售的反相十八烷基硅烷键合硅胶柱(Bond-Elut C18,容量2.8 ml)。CBZ和CBZ-EP的分离通过反相色谱法实现,流动相由乙腈-甲醇-水(19:37:44)组成,流速为1.8 ml/min,结合Nova-Pak C18柱使用。呈径向柱形式的分析柱与Z模块RCSS联用,并由含有Guard-Pak μ Bondapak C18插入物的Guard-Pak预柱模块保护。使用214 nm紫外检测,仅分别用250微升血浆和500微升唾液即可测定CBZ和CBZ-EP浓度在50 - 100 ng/ml范围内。该方法已用于测定接受CBZ单一疗法的儿科患者中药物及其代谢物的稳态浓度,也适用于药代动力学研究。

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