程序可变波长HPLC法测定阿酚咖敏片中4种有效成分及不确定度评定

目的:建立测定阿酚咖敏片中阿司匹林、对乙酰氨基酚、咖啡因与马来酸氯苯那敏含量的方法,并对测量结果进行不确定度评价。方法:采用程序可变波长高效液相色谱法,以乙腈(A)-4.2%磷酸溶液(B)为流动相,梯度洗脱;分析测定过程和步骤,量化各分量的相对标准不确定度。结果:除色谱仪本身的不确定度分量外,方法的准确性、对照品的纯度、称量的大小、样品测量的重复性、稀释过程对合成不确定度贡献较大。阿酚咖敏片样品含量分析中阿司匹林、对乙酰氨基酚、咖啡因和马来酸氯苯那敏相对扩展不确定度分别为1.8%、1.8%、2.0%、2.8%。结论:以马来酸氯苯那敏的不确定度最大;在试验方法的开发中应注意方法的准确性考察;样品测量方面应注意样品的均匀性和样品处理操作过程的一致性,稀释样品时应尽可能地减少稀释步骤。本次评价为提高阿酚咖敏片中有效成分含量测定的可信度提供了一种数学判断方法,对阿酚咖敏片的质量控制具有指导意义。

Determination of 4 Components in Afenkamin Tablets by Programmed-wavelength HPLC and Uncertainty Evaluation

OBJECTIVE： To develop a method for the content determination of aspirin, paracetamol, caffeine and chlorphena- mine maleate in Afenkamin tablets, and to evalute the uncertainty of results. METHODS： The programmed-wavelength HPLC was adopted with acetonitrile （A）-4.2% phosphoric acid solution （B） as mobile phase （gradient elution） ; the procedure and steps of measurement were analyzed, and relative standard uncertainty of components were quantified. RESULTS： Besides the uncertainty of chromatographic instrument, the influential factors of uncertainty contained the accuracy of method, the purity of substance con- trol, sampling amount, the repeatability of sample measurement, elution procedure. The relative expanded uncertainty of aspirin, paracetamol, caffeine and chlorphenamine maleate in Afenkamin tablets were 1.8%, 1.8%, 2.0% and 2.8%, respectively. CON- CLUSIONS ： The uncertainty of chlorphenamine maleate is most significant; the accuracy of the method should be investigated dur- ing the development of experiment method; the homogeneity of sample and sample processing procedure should be considered in the field of sample determination; the steps of elution should be reduced as much as possible. The evaluation of uncertainty pro- vides a mathematical judgment method for improving the credibility of content determiation of effective components in Afenkamin tablets. The method has a certain practical significance on quality control for Afenkamin tablets.