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用于快速测定卡马西平(“痛惊宁”)的三甲基硅烷基(TMS)衍生物的等温气相色谱法。

Isothermal gas chromatographic method for the rapid determination of carbamazepine ("tegretol") as its TMS derivative.

作者信息

Lensmeyer G L

出版信息

Clin Toxicol. 1977;11(4):443-54. doi: 10.3109/15563657708988208.

DOI:10.3109/15563657708988208
PMID:589957
Abstract

A rapid, simple isothermal gas chromatographic (GC) method for the quantitation of carbamazepine ("Tegretol") in serum as its trimethylsilyl derivative has been developed. A single chloroform extraction using 1.0 ml of serum, a 10-min derivatization step, and analysis on a 3% OV-1 (methyl silicone) GC column gives a linear response to a carbamazepine concentration up to 25 mg/liter. A non-drug internal standard (tetracosane) compensates for variables in extraction, injection, and instrumental changes occurring during analysis. This method was found to be free of interferences from endogenous substances in the serum, as well as from toxic concentrations of commonly used drugs. Day-to-day precision at concentration levels of 2, 5, and 10 mg/liter ranged from 2.9 to 4.4% (CV). Standard addition studies of carbamazepine added to serum resulted in a mean recovery of 95%. To ensure accurate results, all standards were prepared in serum.

摘要

已开发出一种快速、简单的等温气相色谱(GC)方法,用于定量测定血清中作为其三甲基硅烷基衍生物的卡马西平(“ Tegretol”)。使用1.0 ml血清进行单次氯仿萃取、10分钟衍生化步骤,并在3% OV-1(甲基硅氧烷)GC柱上进行分析,对高达25 mg/升的卡马西平浓度给出线性响应。一种非药物内标(二十四烷)可补偿分析过程中萃取、进样和仪器变化的变量。该方法被发现不受血清中内源性物质以及常用药物中毒性浓度的干扰。在2、5和10 mg/升浓度水平下的日常精密度范围为2.9%至4.4%(CV)。向血清中添加卡马西平的标准加入研究结果显示平均回收率为95%。为确保结果准确,所有标准品均在血清中制备。

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