阿替洛尔、美托洛尔和普萘洛尔高效液相色谱分析的误差结构：参数估计中的一种有效加权方法。

Error structure for the HPLC analysis for atenolol, metoprolol and propranolol: a useful weighting method in parameter estimation.

作者信息

Modamio P, Lastra C F, Mariño E L

机构信息

Department of Pharmacy, Faculty of Pharmacy, University of Barcelona, Spain.

出版信息

J Pharm Biomed Anal. 1998 Jul;17(3):507-13. doi: 10.1016/s0731-7085(97)00236-7.

DOI:10.1016/s0731-7085(97)00236-7

PMID:9656163

Abstract

Three reversed-phase high performance liquid chromatography (HPLC) methods with UV detection were developed and fully validated for the quantification of three beta-blockers: atenolol, metoprolol and propranolol. After validation, error structures for the HPLC analysis were established using a convenient and practical procedure. The mean percentage of relative standard deviation (RSD) of the experimental concentrations (C), were less than 4.29% for proportionality and less than 3.68% for precision for any of the drugs, which allowed the quantitation of beta-blockers assayed at concentrations in the range 25-0.78 micrograms.ml-1. The error structures for the HPLC analysis were: SD (micrograms.ml-1) = 5.02 x 10(-2) C for atenolol, SD (micrograms.ml-1) = 4.55 x 10(-2) + 0.63 x 10(-2) C - 7.58 x 10(-6) C3 for metoprolol and SD (micrograms.ml-1) = 2.73 x 10(-2) C - 3.49 x 10(-4) C2 for propranolol. The reciprocal of the square of the SD of the drug concentrations measured within the calibration curve could be used as weighting methods in parameter estimation by non-linear regression.

摘要

开发了三种带紫外检测的反相高效液相色谱（HPLC）方法，并对三种β受体阻滞剂：阿替洛尔、美托洛尔和普萘洛尔进行了全面验证以进行定量分析。验证后，采用一种简便实用的程序建立了HPLC分析的误差结构。实验浓度（C）的相对标准偏差（RSD）平均百分比，对于任何一种药物，比例方面小于4.29%，精密度方面小于3.68%，这使得能够对浓度范围在25 - 0.78微克·毫升-1的β受体阻滞剂进行定量分析。HPLC分析的误差结构为：阿替洛尔的SD（微克·毫升-1） = 5.02×10(-2)C；美托洛尔的SD（微克·毫升-1） = 4.55×10(-2) + 0.63×10(-2)C - 7.58×10(-6)C3；普萘洛尔的SD（微克·毫升-1） = 2.73×10(-2)C - 3.49×10(-4)C2。在校准曲线内测得的药物浓度标准差平方的倒数可作为非线性回归参数估计中的加权方法。