摘要
首次建立高效液相色谱-紫外检测(HPLC-UV)双波长法测定丁苯那嗪原料药中7个有关物质。采用Welch Ultimate XB-C18色谱柱,以0.005 mol/L磷酸氢二钾和0.005 mol/L磷酸二氢钾溶液(pH 7.0)为流动相A,乙腈为流动相B,梯度洗脱,检测波长为284 nm、220 nm。结果表明,各有关物质在0.5~10.0μg/ml内线性关系良好,方法回收率为90%~108%。建立的方法灵敏度好、选择性强、重复性好。此外,通过质谱与核磁共振鉴定了未知氧化降解杂质(有关物质B)的结构为1-羟基-3-异丁基-9,10-二甲氧基-1,3,4,6,7,11b-六氢吡啶并[2,1-α]异喹啉-2-酮。
An high performance liquid chromatography-ultraviolet detection method(HPLC-UV)with dualwavelength was established for the determination of seven related substances in tetrabenazine.A Welch Ultimate XBC18 chromatographic column was used,with 0.005 mol/L dipotassium hydrogen phosphate and 0.005 mol/L potassium dihydrogen phosphate solution(pH 7.0)as mobile phase A,and acetonitrile as mobile phase B(gradient elution).The detection wavelengths were 284 nm and 220 nm.The results showed that it was linear for the related substances in the range of 0.5~10.0μg/ml.The recoveries were 90%~108%.The sensitivity,selectivity and repeatability of this method were good.In addition,the unknown oxidative degradation impurity(related substance B)was identified by mass spectrometry and nuclear magnetic resonance as 1-hydroxy-3-isobutyl-9,10-dimethoxy-1,3,4,6,7,11b-hexahydropyrido[2,1-α]isoquinoline-2-ketones.
作者
徐桂丽
周爱南
何奇
万博
张庆伟
XU Guili;ZHOU Ainan;HE Qi;WAN Bo;ZHANG Qingwei(College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science,Shanghai 201620;Novel Technology Center of Pharmaceutical Chemistry,Shanghai Institute of Pharmaceutical Industry,China State Institute of Pharmaceutical Industry,Shanghai 201203;Shanghai Engineering Research Center of Pharmaceutical Process,Shanghai 201203;Jilin Aodong Taonan Pharmaceutical Co.,Ltd.,Taonan 137100)
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2021年第1期120-130,共11页
Chinese Journal of Pharmaceuticals
