高效液相色谱法测定盐酸可乐定中有机杂质的含量  

Determination of organic impurities in clonidine hydrochloride by HPLC

作　　者：刘慧颖 张耀文 蒋丹丹 隋晓璠 孙苓苓 LIU Hui-ying;ZHANG Yao-wen;JIANG Dan-dan;SUI Xiao-fan;SUN Ling-ling(Liaoning Institute for Drug Control,Liaoning Inspection,Testing and Certification Center,State Key Laboratory of Chemical Drug Quality Research and Evaluation,Shenyang 110023)

机构地区：[1]辽宁省药品检验检测院,辽宁省检验检测认证中心,化学药品质量研究与评价国家重点实验室,沈阳110023

出　　处：《中南药学》2022年第7期1644-1648,共5页Central South Pharmacy

基　　金：国家药典委员会2020年国家药品标准提高研究(No.2020H031);辽宁省自然基金资助计划(No.2020-MS-074)。

摘　　要：目的对盐酸可乐定有机杂质进行分析和测定,对两家企业的原料质量进行考察。方法结合工艺和影响因素试验结果,建立适合分析有机杂质的HPLC方法,并进行验证。确定选用Waters C8色谱柱,0.22%辛烷磺酸钠-甲醇-磷酸(600∶400∶1,用1 mol·L^(-1)氢氧化钠溶液调节pH值至3.0)为流动相,紫外检测波长为220 nm。结果杂质A、杂质B、2,6-二氯苯胺的线性范围分别为2.29~18.29 ng(r=1.000)、2.22~17.79 ng(r=1.000)和2.29~18.33 ng(r=1.000);平均回收率分别为96.51%、100.31%和91.29%,重复性考察的RSD分别为1.5%、1.0%和2.8%。两家企业原料药均未检出有机杂质。结论该方法可用于盐酸可乐定的药品质量控制。Objective To determine and analyze the organic impurities in clonidine hydrochloride,and investigate the quality of raw materials from two manufacturers.Methods A suitable HPLC method for analyzing organic impurities was established and verified based on the synthesis process and influence factor investigation.Organic impurities were separated on a Waters C8 column,the ternary mobile phase consisting of 0.22%sodium octane sulfonate-methanol-phosphoric acid(600∶400∶1,pH was adjusted to 3.0 with 1 mol·L^(-1) sodium hydroxide solution),and the detection wavelength was 220 nm.Results The linear calibration curves were obtained at 2.29~18.29 ng for impurity A,2.22~17.79 ng for impurity B,and 2.29~18.33 ng for 2,6-dichloroaniline,respectively.The mean recoveries of the three compounds were 96.51%,100.31%and 91.29%,and the RSDs of repeatability were 1.5%,1.0%and 2.8%,respectively.No organic impurities were detected in the raw materials from two manufcturers.Conclusion This method can be used for the quality control of clonidine hydrochloride.

关 键 词：有机杂质 杂质A 杂质B 2 6-二氯苯胺 盐酸可乐定 

分 类 号：R927.2[医药卫生—药学]