HPLC法同时测定复方苯硝那敏片中4种成分的含量

HPLC simultaneous determination of phenobarbital,nitrazepam,vitamin B_6 and chlorphenamine maleate in compound phenobarbital nitrazepam and chlorphenamine tablets

目的:为控制复方苯硝那敏片质量,建立高效液相色谱法同时测定复方苯硝那敏片中苯巴比妥、硝西泮、维生素B6及马来酸氯苯那敏的含量。方法:选用C18柱IntersilODS-3(4.6mm×250mm,5μm),甲醇-0.01mol·L-1醋酸铵(含0.1%冰醋酸)梯度洗脱,流速:1mL·min-1,检测波长:254nm;进样量:20μL;柱温:35℃。结果:本方法可同时测定复方苯硝那敏片中上述4种主要成分的含量,对复方苯硝那敏片的质量进行控制。苯巴比妥在0.2983～0.5966mg·mL-1(r=0.9999)、硝西泮在0.02525～0.05050mg·mL-1(r=0.9999)、马来酸氯苯那敏在0.03958～0.07915mg·mL-1(r=0.9999)、维生素B6在0.0996～0.1992mg·mL-1(r=0.9998)范围内,峰面积与其浓度呈良好的线性关系。平均回收率分别为:苯巴比妥99.5%,RSD=0.2%(n=3);硝西泮100.6%,RSD=0.2%(n=3);马来酸氯苯那敏100.0%,RSD=0.19%(n=3);维生素B6100.5%,RSD=0.2%(n=3)。结论:该方法简便、灵敏、准确,适用于复方苯硝那敏片中各主要成分的含量测定及该品种的质量控制。

Objective：To establish an HPLC method for simultaneous determination of phenobarbital,nitrazepam,vitamin B6 and chlorphenamine maleate in compound phenobarbital nitrazepam and chlorphenamine Tablets.Methods：The HPLC using Intersil ODS-3 C18 column（4.6 mm×250 mm,5 μm）,the mobile phase consisted of methanol-0.01 mol·L-1 ammonium acetate（includeing 0.1% glacial acetic acid）,the flow rate was 1 mL·min-1 and detected at 254 nm,the injection volume was 20 μL,column temperature was 35 ℃.Results：The contents of four components could be simultaneously determined.The calibration curves were linear in the ranges of 0.2983-0.5966 mg·mL-1（r=0.9999）for phenobarbital,0.02525-0.05050 mg·mL-1（r=0.9999）for nitrazepam,0.03958-0.07915 mg·mL-1（r=0.9999）for chlorphenamine maleate,0.0996-0.1992 mg·mL-1（r=0.9998）for vitamin B6.The average recovery of phenobatbital was 99.5%,RSD=0.2%（n=3）,Nitrazepam was 100.6%,RSD=0.2%（n=3）,vitamin B6 was 100.5%,RSD=0.2%（n=3）,chlorphenamine maleate was 100.0%,RSD=0.19%（n=3）.Conclusion：This method is simple,fast,accurate,and can be used to simultaneously determine concentration of phenobarbital,nitrazepam,vitamin B6 and chlorphenamine maleate in compound phenobarbital nitrazepam and chlorphenamine tablets.