HPLC-CAD法测定阿卡波糖胶囊含量

Determination of acarbose capsules by HPLC-CAD

目的:针对目前标准中阿卡波糖含量测定方法灵敏度低、氨基柱柱效流失严重、耐用性差等问题,建立了高效液相色谱-电喷雾检测器(HPLC-CAD)法测定阿卡波糖胶囊的含量。方法:采用Waters XBridge Amide色谱柱(4.6 mm×250 mm,3.5μm),以乙腈--00..22%%三乙胺溶液(70∶30)为流动相,流速为1.0mL·min^-1,柱温45℃;电喷雾检测器参数:雾化温度55℃,幂率1.0,采样频率10 Hz。结果:阿卡波糖与相邻杂质以及各杂质峰间的分离均良好;在0.05~1.0 mg·mL^-1范围内线性关系良好(R^2=0.9994);阿卡波糖高、中、低3种浓度的回收率分别为99.2%、100.7%和99.6%。5批样品中阿卡波糖的含量分别为100.1%、100.2%、99.5%、98.6%和100.4%,经t检验统计分析,P>0.05,表明建立的HPLC-CAD法与《中华人民共和国药典》收载的方法无显著性差异。结论:HPLC-CAD法操作简单,专属性强,灵敏度高,色谱柱柱效好,耐用性强,弥补了目前标准中阿卡波糖含量测定方法的不足,可作为阿卡波糖胶囊质量控制和评价的新方法。

Objective:To establish an HPLC-CAD method for determination of content of acarbose capsules in order to solve the problems of the poor sensitivity and durability of the present method for the detection of acarbose with amino column in the domestic pharmacopoeia.Methods:A Waters XBridge Amide column(4.6 mm×250 mm,3.5μm)was used.The mobile phase was composed of acetonitrile-0.2%triethylamine aqueous solution(70∶30)at the flow rate of 1.0 mL·min^-1 and the column temperature was maintained at 45℃.The detector of CAD was applied with the nebulization temperature of 55℃,collection frequency of 10 Hz and power function value(PFV)of 1.0.Results:Acarbose and all impurities were well separated by this method.The linearity of acarbose was fine in the range of 0.05-1.0 mg·mL^-1 with the correlation coefficient square of 0.9994.The recoveries of acarbose were 99.2%,100.7%and 99.6%at high,medium and low concentrations,respectively.Acarbose content of five batches of capsule samples was 100.1%,100.2%,99.5%,98.6%and 100.4%,respectively.The results of the five batches of samples showed P>0.05 which were analyzed by t test.The data indicated that the HPLC-CAD method and HPLC-UV method had no significant difference,and the established HPLC-CAD method could replace the HPLC-UV method.Conclusion:Compared to the present method,the established HPLC-CAD method showed better convenience,sensitivity and robustness and can make up the defects of the present method in the domestic pharmacopoeia,which could be a reliable method for the quality control of acarbose capsules.