HPLC双波长法同时测定复方羟丙茶碱去氯羟嗪胶囊中5个成分  

Simultaneous determination of five components in diprophylline,bromhexine hydrochloride,decloxizine hydrochloride,raceanisodamine and clenbuterol hydrochloride capsules by double-wavelength HPLC

作　　者：鲁辉 吴杨 许奇 钱岩 黄逸文 LU Hui;WU Yang;XU Qi;QIAN Yan;HUANG Yi-wen(Suzhou Institute for Drug Control Suzhou Centre of Adverse Drug Reaction Monitoring,Suzhou 215000,China)

机构地区：[1]苏州市药品检验检测研究中心苏州市药品不良反应监测中心,苏州215000

出　　处：《药物分析杂志》2023年第2期245-252,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC双波长法同时测定复方羟丙茶碱去氯羟嗪胶囊中二羟丙茶碱、盐酸去氯羟嗪、盐酸溴己新、消旋山莨菪碱、盐酸克伦特罗5个活性成分的含量。方法:采用Zorbax Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm),以0.01 mol·L^(-1)磷酸二氢钾溶液(加离液盐:0.05 mol·L^(-1)的高氯酸钠作为添加剂,磷酸调pH至2.5)为流动相A,乙腈为流动相B,梯度洗脱,流速1.0 mL·min^(-1),采用240 nm(二羟丙茶碱、盐酸去氯羟嗪、盐酸溴己新)和210 nm(消旋山莨菪碱、盐酸克伦特罗)的双波长作为检测波长,进样量20μL,柱温35℃。结果:二羟丙茶碱、盐酸去氯羟嗪、盐酸溴己新、消旋山莨菪碱、盐酸克伦特罗5个成分在2种波长下均达到完全分离;拖尾因子均<1.5;各成分质量浓度在相应范围内与峰面积呈良好线性关系;重复性RSD(n=6)分别为0.25%、0.50%、0.18%、0.77%、1.8%;各成分低、中、高3个加标水平下平均回收率(n=3)分别为100.7%~101.0%、100.0%~101.5%、100.4%~101.5%、99.8%~102.4%、97.6%~101.9%。3批样品中5个成分的含量分别为标示量的100.6%~101.4%、100.0%~100.9%、98.7%~98.9%、97.9%~98.2%、91.5%~92.4%。结论:建立的方法可同时测定复方羟丙茶碱去氯羟嗪胶囊中全部5个活性成分,且方法简便准确,完善了其质量控制与评价体系;由于这5个成分也是其他止咳平喘类复方制剂中的常见活性成分,因此该方法也为其他复方制剂同时测定其中多个成分提供了借鉴。Objective:To establish a double-wavelength HPLC method for simultaneous determination of all 5 active ingredients in diprophylline,bromhexine hydrochloride,decloxizine hydrochloride,raceanisodamine and clenbuterol hydrochloride capsules.Methods:The method was performed on a Zorbax Eclipse XDB-C18column(250 mm×4.6 mm,5μm).The mobile phases consisted of A(0.01 mol·L^(-1)potassium dihydrogen phosphate solution with the chaotropic salt:0.05 mol·L^(-1)sodium perchlorate as additive,adjusted to pH 2.5 with phosphoric acid)and B(acetonitrile)in gradient mode at a flow rate of 1.0 mL·min^(-1).The detective wavelengthwas set at 240 nm for diprophylline,bromhexine hydrochloride and decloxizine hydrochloride while 210 nm for raceanisodamine and clenbuterol hydrochloride.The injection volume was 20μL and the column temperature was 35℃.Results:The five components of diprophylline,bromhexine hydrochloride,decloxizine hydrochloride,raceanisodamine and clenbuterol hydrochloride were separated well at the both wavelength with the tailing factor below 1.5 and indicated good linearity between peak areas and concentration.RSD of the repeatability tests(n=6)were 0.25%,0.50%,0.18%,0.77%and 1.8%while the average recoveries(n=3)at the low,medium and high spiked levels were 100.7%-101.0%,100.0%-101.5%,100.4%-101.5%,99.8%-102.4%and 97.6%-101.9%respectively.The contents of the five components in three batches of samples were 100.6%-101.4%,100.0%-100.9%,98.7%-98.9%,97.9%-98.2%and 91.5%-92.4%of the labeled amount respectively.Conclusion:This method proved simple and accurate for simultaneous determination of all five active ingredients,which can be used for quality control and evaluation of this preparation.The method also provides an example to simultaneous determination for the relative active ingredients in other preparations since the five components were common in cough medicine.

关 键 词：二羟丙茶碱 盐酸去氯羟嗪 盐酸溴己新 消旋山莨菪碱 盐酸克仑特罗 离液盐 高效液相色谱双波长法 

分 类 号：R917[医药卫生—药物分析学]