三种呼吸系统兽药制剂中非法添加盐酸溴己新、吲哚美辛的HPLC-PDA检测方法的建立

Determination of Bromhexine Hydrochloride and Indometcain Illegally Added in Three Veterinary Preparations by HPLC-PDA

关键词:  盐酸溴己新  吲哚美辛  麻杏石甘散  氟苯尼考注射液  甘草颗粒

Key words:  Bromhexine Hydrochloride  Indometcain  Maxing Shigan Power  Florfenicol Injection  Gancao Granule

摘要:

为检测麻杏石甘散、氟苯尼考注射液中非法添加的盐酸溴己新,甘草颗粒中非法添加的吲哚美辛,以十八烷基键合硅胶为填充剂,磷酸盐缓冲液-乙腈(20:80)为流动相检测盐酸溴己新,以乙腈-0.1mol/L冰醋酸溶液(50∶50)为流动相检测吲哚美辛,流速为1.0 ml/min,波长扫描范围为200～400 nm,建立了相应的HPLC-PAD检测方法,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。结果显示,盐酸溴己新在麻杏石甘散中和氟苯尼考注射液中的回收率分别为94.8%和 98.5%,吲哚美辛在甘草颗粒中回收率为95.2%；盐酸溴己新线性方程为y=14780200x-16476,R=0.9999,吲哚美辛线性方程为y=10995430x+13033,R=0.9999；麻杏石甘散中盐酸溴己新检测限为83 mg/kg,氟苯尼考注射液中盐酸溴己新检测限为1.6 g/L,甘草颗粒中吲哚美辛检测限为1 g/kg。

Abstract:

Methods for the determination of Bromhexine Hydrochloride in Maxing Shigan Power and Florfenicol Injection as well as Indometcain in Gancao Granule were developed by the high performance liquid chromatography with photo-diode array detector(HPLC-PDA).It was tested with C18 column, using phosphate buffer and acetonitrile(20:80),0.1mol/L acetic acid and acetonitrile(50:50)as the mobile phases. The scanning wavelength was from 200nm to 400nm.Peak purity test and spectrum similarity test were used to identify Bromhexine Hydrochloride and Indometcain. The mean recoveries of Bromhexine Hydrochloride in Maxing Shigan Power and Florfenicol Injection were 94.8% and 98.5%. The mean recovery of Indometcain in Gancao Granule was 95.2%. In conclusion, the method is simple, accurate and reliable for the determination of Bromhexine Hydrochloride and Indometcain in those three veterinary preparations.