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血清中普萘洛尔的灵敏高效液相色谱分析法

A sensitive high-performance liquid chromatographic analysis of propranolol in serum.

作者信息

al-Angary A A, el-Sayed Y M, al-Meshal M A, al-Dardiri M M, Mahrous G M

机构信息

Department of Pharmaceutics, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia.

出版信息

J Clin Pharm Ther. 1991 Apr;16(2):93-101. doi: 10.1111/j.1365-2710.1991.tb00289.x.

Abstract

A rapid and sensitive high-performance liquid chromatographic (HPLC) assay was developed for quantitative determination of propranolol in serum. The assay is performed after single extraction of propranolol and indenolol [internal standard (IS)] from alkalinized serum into ether and eluted from C-18 U Bondapak column with a mobile phase composed of methanol: 0.01 M phosphate buffer pH 3.4 (40:60%, v/v). The column eluant was monitored on a fluorescence detector. Measurement was achieved by taking the peak height ratio of propranolol and comparing it to that of the IS. The detection limit for propranolol in serum is 2.5 ng/ml. Intraday coefficients of variation (CV) ranged from 2.84 to 4.0% and interday (CVs) from 5.8 to 8.4% at three different concentrations. The relative and absolute recoveries varied from 93.8 to 102.3%. Preliminary stability tests showed that propranolol is stable for at least 3 weeks in serum after freezing. The method is applied for the determination of the pharmacokinetic parameters of propranolol after intravenous administration (1 mg/kg) to rabbits.

摘要

建立了一种快速灵敏的高效液相色谱(HPLC)法,用于定量测定血清中的普萘洛尔。该方法是将普萘洛尔和茚萘洛尔[内标(IS)]从碱化血清中单次萃取到乙醚中,然后用由甲醇:0.01 M pH 3.4的磷酸盐缓冲液(40:60%,v/v)组成的流动相从C-18 U Bondapak柱上洗脱。柱洗脱液在荧光检测器上进行监测。通过测定普萘洛尔的峰高比并与内标的峰高比进行比较来实现测定。血清中普萘洛尔的检测限为2.5 ng/ml。在三种不同浓度下,日内变异系数(CV)范围为2.84%至4.0%,日间变异系数(CV)范围为5.8%至8.4%。相对回收率和绝对回收率在93.8%至102.3%之间。初步稳定性试验表明,普萘洛尔在冷冻后的血清中至少稳定3周。该方法用于测定家兔静脉注射(1 mg/kg)普萘洛尔后的药代动力学参数。

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