RP-HPLC法测定氯磺丙脲有关物质方法的建立  

RP-HPLC determination of the related substances in chlorpropamide

作　　者：周建玉[1] 唐素芳[1] 

机构地区：[1]天津市药品检验所,天津300070

出　　处：《药物分析杂志》2010年第9期1788-1791,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：中国药典2010版药典科研课题

摘　　要：目的:建立RP-HPLC法测定氯磺丙脲有关物质。方法:采用Waters2695型高效液相色谱仪,色谱柱为KromasilC18(4.6mm×250mm,5μm)色谱柱,流动相为乙腈-磷酸二氢铵溶液(取磷酸二氢铵1.725g,加水300mL使溶解,用磷酸调节pH至3.50±0.05)(625∶375),流速1.0mL.min-1,检测波长200nm。结果:氯磺丙脲与其相关杂质分离度良好,浓度在0.15～7.5μg·mL-1范围内与峰面积呈良好的线性关系(r=0.9999,n=6);已知杂质4-氯苯磺酰胺的相对响应因子为0.86,1,3-二丙基脲的相对响应因子为3.9;氯磺丙脲最低检出量为3ng。结论:本方法专属性好,灵敏度高,结果准确,可用于氯磺丙脲质量控制。Objective：To establish an RP-HPLC method for the analysis of the related substances in chlorpropamide.Method：The RP-HPLC method was performed on a Waters 2695 liquid chromatography and coupled UV detector at 200 nm.Kromasil C18 column（4.6 mm×250 mm,5 μm） was adopted with the mobile phase of acetonitrile-ammonium dihydrogen phosphate solute／[adjusted pH to 3.50±0.05 by phosphoric acid／]（625：375） at a flow rate of 1.0 mL·min-1.Results：The resolution between chlorpropamide and related substances was satisfied.A linearity between peak area and chlorpropamide concentration was achieved in the range of 0.15-7.5 μg·mL-1 with r of 0.9999（n=6）.The relative response factor of impurity A（4-chlorobenzenesulfonamide） and impurity B（1,3-dipropylurea） were 0.86 and 3.9,respectively.The LOD of chlorpropamide was 3 ng.Conclusion：The method is accurate,specific,and sensitive and can be used for quality control of chlorpropamide.

关 键 词：氯磺丙脲 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]