HPLC法同时测定茶新那敏薄膜包衣片中三组分的含量

HPLC simultaneous determination of three kinds of ingredients in aminophylline bromhexine and chlorphenamine membrane coat tablets

目的:建立HPLC法同时测定茶新那敏薄膜包衣片中茶碱、盐酸溴己新和马来酸氯苯那敏的含量。方法:采用ZORBAXExtend-C18(25 cm×4.6 mm,5μm)色谱柱;以甲醇-乙腈-0.017 mol·L-1高氯酸液[取高氯酸(70%～72%)2.4 mL,加水1000 mL,用三乙胺调节pH至3.5±0.02](45∶5∶50)为流动相;流速1.0 mL·min-1;检测波长220 nm;进样量为10μL;柱温:30℃。结果:茶碱浓度在75.28～752.8μg·mL-1之间、盐酸溴己新浓度在16.12～161.2μg·mL-1之间、马来酸氯苯那敏浓度在1.488～14.88μg·mL-1之间均与峰面积呈良好线性关系,r=0.9993～1.000;茶碱、盐酸溴己新、马来酸氯苯那敏低、中、高3个浓度平均加样回收率分别为100.1%～101.5%,98.0～101.0%,99.6%～102.7%;平均回收率分别为100.7%(RSD=0.72%),99.4%(RSD=1.5%),101.0%(RSD=1.6%)。结论:本法操作简便,结果准确,可作为该制剂的质量控制方法。

Objective：To establish an HPLC method for simultaneous determination of theophylline,bromhexine hydrochloride and chlorphenamine maleate in aminophylline bromhexine and chlorphenamine membrane coat tablets.Methods：The HPLC method was performed in the following modules.The sample was separated and analyzed on ZORBAX Extend-C18（25 cm×4.6 mm,5 μm）column,and methanol-acetonitrile-0.017 mol·L-1 perchloric acid solution [to 2.4 mL of perchloric acid（70%-72%）,add 1000 mL of water,adjusted pH to 3.5±0.02 with triethylamine]（45∶ 5∶ 50） was used as mobile phase.The flow rate was at 1.0 mL·min-1,the detective wavelength was at 220 nm,the injection volume was 10 μL,and the column temperature was 30 ℃.Results：The theophylline,bromhexine hydrochloride and chlorphenamine maleate peaks in the sample chromatogram were completely separated from other ingredient peaks.The calibration curve was linear at a range of 75.28-752.8 μg·mL-1for theophylline with r=0.9993,of 16.12-161.2 μg·mL-1 for bromhexine hydrochloride with r=1.000 and of 1.488-14.88 μg·mL-1 for chlorphenamine membrane with r=0.9993.The average recoveries（n=3） of theophylline samples at low,moderate and high concentrations were between 100.1%-101.5% with an average recovery of 100.7%（RSD=0.72%）;of bromhexine hydrochloride were between 98.0%-101.0%,with an average recovery of 99.4%（RSD=1.5%）;of chlorphenamine maleate were between 99.6%-102.7%,with an average recovery of 101.0%（RSD=1.6%）.Conclusion：This method is simple and accurate,which can be used for quality control of this preparation.