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采用带紫外检测器的反相高效液相色谱法测定人血浆中克林霉素的简易方法。

Simple method for the assay of clindamycin in human plasma by reversed-phase high-performance liquid chromatography with UV detector.

作者信息

Cho Sung-Hee, Im Ho-Taek, Park Wan-Su, Ha Yong-Hwa, Choi Young-Wook, Lee Kyung-Tae

机构信息

College of Pharmacy, Kyung-Hee University, Hoegi-dong, Dongdaemun-ku, Seoul, 130-701, Korea.

出版信息

Biomed Chromatogr. 2005 Dec;19(10):783-7. doi: 10.1002/bmc.517.

Abstract

A rapid and simple high-performance liquid chromatography (HPLC) method was developed and validated for the quantification of clindamycin in human plasma. After precipitation with 50% trichloroacetic acid (TCA) containing the internal standard, propranolol, the analysis of the clindamycin level in the plasma samples was carried out using a reverse-phase cyano (CN) column with ultraviolet detection (204 nm). The chromatographic separation was accomplished with an isocratic mobile phase consisting of acetonitrile-distilled water-7.6 mm tetramethylammonium chloride (TMA) (60:40:0.075, v/v/v), adjusted to pH 3.2. The proposed method was specific and sensitive with a lower limit of quantitation (LLOQ) of 0.2 microg/mL. This HPLC method was validated by examining the precision and accuracy for inter- and intraday analysis in the concentration range 0.2-20.0 microg/mL. The relative standard deviations (RSD) in the inter- and intraday validation were 6.1-14.9 and 6.0-16.1%, respectively. In the stability test, clindamycin was found to be stable in human plasma during the storage and assay procedure. The present HPLC method was applied to the analysis of samples taken up to 12 h after a single oral administration of clindamycin in healthy volunteers.

摘要

建立并验证了一种快速简便的高效液相色谱(HPLC)法,用于定量测定人血浆中的克林霉素。在用含内标普萘洛尔的50%三氯乙酸(TCA)沉淀后,使用带有紫外检测(204 nm)的反相氰基(CN)柱对血浆样品中的克林霉素水平进行分析。色谱分离采用等度流动相,该流动相由乙腈-蒸馏水-7.6 mM四甲基氯化铵(TMA)(60:40:0.075,v/v/v)组成,pH值调至3.2。所提出的方法具有特异性和灵敏性,定量下限(LLOQ)为0.2 μg/mL。通过考察0.2 - 20.0 μg/mL浓度范围内日间和日内分析的精密度和准确度,对该HPLC法进行了验证。日间和日内验证中的相对标准偏差(RSD)分别为6.1 - 14.9%和6.0 - 16.1%。在稳定性试验中,发现克林霉素在人血浆的储存和分析过程中是稳定的。本HPLC法应用于健康志愿者单次口服克林霉素后长达12小时采集的样品分析。

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