高效液相色谱法测定琥珀酸多西拉敏片中有关物质  

Determination of related substances in doxylamine succinate tablets by HPLC

作　　者：乔乔 余小红 陈斌[1] 晏飞 曹阳 黄顺旺 曹明成[1] QIAO Qiao;YU Xiaohong;CHEN Bin;YAN Fei;CAO Yang;HUANG Shunwang;CAO Mingcheng(Hefei Innovative Pharmaceutical Technology Co.,Ltd.,Hefei,Anhui 230088,China)

机构地区：[1]合肥创新医药技术有限公司,安徽合肥230088

出　　处：《安徽医药》2020年第10期1958-1961,共4页Anhui Medical and Pharmaceutical Journal

基　　金：合肥市2018年省战略性新兴产业集聚发展基地研发类项目(11)。

摘　　要：目的建立高效液相色谱法(HPLC)法测定琥珀酸多西拉敏片中的有关物质。方法2017年10月至2018年9月,采用高效液相色谱法,紫外检测器,苯基硅烷键合硅胶柱,固定相:Polar-Phenyl,250 mm×4.6 mm,5μm,流动相:0.01 mol/L磷酸二氢钾溶液(加三乙胺溶液3 m L,用磷酸调节p H至3.0)-乙腈(89∶11),检测波长:260 nm。结果5种已知杂质和琥珀酸多西拉敏及其他未知杂质均能得到有效分离;琥珀酸多西拉敏、杂质A、B、C、E和G分别在0.08~20.36、0.08~20.14、0.05~19.85、0.10~20.66、0.25~20.39、0.05~22.63μg/mL范围内线性关系良好,r均为0.9999。杂质A、B、C、E和G平均回收率分别为99.62%,98.87%,101.68%,102.85%和100.41%。结论本方法灵敏、准确、可靠,能够准确测定琥珀酸多西拉敏片的有关物质。Objective To establish a HPLC method for determining the related substances in doxylamine succinate tablets.MethodsHigh performance liquid chromatography,ultraviolet detector and phenylsilane bonded silica gel column were used from Octo-ber 2017 to September 2018.Stationary phase was Polar-Phenyl(250 mm×4.6 mm,5μm),mobile phase consisted water of 0.01 mol·L-1 potassium dihydrogen phosphate(add 3 m L of triethylamine and adjusted p H to 3.0 with phosphoric acid)-acetonitrile(89∶11).The detective wavelength was set at 260 nm.ResultsDoxylamine succinate and its five related substances(impurity A,B,C,E andG)were determinated by HPLC,in which the linearity were good within the range 0.08-20.36,0.08-20.14,0.05-19.85,0.10-20.66,0.25-20.39 and 0.05-22.63μg/m L,and the regression coefficient were all 0.9999,respectively,while the recoveries of the five relat-ed substances were 99.62%,98.87%,101.68%,102.85%and 100.41%.ConclusionThis method was operated easily,and it canbe used to accurately determinate the related substances contend in doxylamine succinate tablets.

关 键 词：多西拉敏/分析 色谱法 高压液相 药物污染 回收率 

分 类 号：R927.2[医药卫生—药学]