摘要
目的建立一种测定聚多卡醇注射液有关物质和聚多卡醇含量的方法。方法采用高效液相色谱-示差折光检测器法进行测定。色谱柱为Nucleosil-120C18柱(250mm×4mm,5μm)或效能相当的色谱柱;流动相为乙腈-甲醇-水=20∶68∶12;流速为1.0ml/min;柱温和检测器温度均为45℃;进样量为20μl。按不加校正因子的主成分自身对照法测定聚多卡醇注射液中的已知杂质[正十二醇、C10(EO)nOH、C14(EO)nOH]和未知杂质,采用外标法测定聚多卡醇注射液中聚多卡醇的含量。结果有关物质中主成分检测质量浓度线性范围为2.7316~109.2638μg/ml(r=0.99997),相应的杂质限度范围为0.05%~2.00%,检测限为0.6829μg/ml。聚多卡醇含量测定中主成分检测质量浓度线性范围为0.98~2.93mg/ml(r=0.99996),平均回收率为99.3%(RSD=0.9%,n=9)。测定两个规格6批聚多卡醇注射液样品的含量分别为100.6%、101.3%、102.0%、100.1%、100.8%、101.2%。结论本文建立的聚多卡醇注射液中的聚多卡醇含量和有关物质测定方法,简单可行,可有效控制聚多卡醇注射液的质量。
Objective To establish a method for the determination of related substances and Polidocanol contents in Polidocanol Injection.Methods The method of high performance liquid chromatography-differential refractive index detector method was adopted.The determination was performed on a Nucleosil-120 C18 column (250 mm×4 mm,5 μm),or a chromatographic column of comparable potency;the mobile phase consisted of acetonitril-methanol-water was 20∶68∶12;the flow rate was 1.0 ml/min;the temperatures of both the column and the detector were 45℃;the injection volume was 20 μl.The known impurities,such as n-dodecyl alcohol,C10(EO)nOH,C14(EO)nOH),and unknown impurities in Polidocanol Injection were determined by principal component self-control method without correction factor,and the Polidocanol contents of Polidocanol Injection was determined by external standard method.Results The linear range of main component in related substances test were 2.7316-109.2638 μg/ml (r=0.99997),and the limits of related impurity were 0.05%-2.0%,the detection limits was 0.6829 μg/ml.The linear range of main component in polidocanol content test were 0.98-2.93 mg/ml (r=0.99996),the rate of average recovery was 99.3%(RSD=0.9%,n=9).The contents of 6 batches of Polidocanol Injection samples were determined as 100.6%,101.3%,102.0%,100.1%,100.8% and 101.2%,respectively.Conclusion The method for determination of Polidocanol contents and related substances in Polidocanol Injection is simple and feasible,which can effectively control the quality of Polidocanol Injection.
作者
杨梅
欧嘉娜
YANG Mei;OU Jia-na(Department of Chemical Office,Guangzhou Institute for Drug Control,Guangdong Province,Guangzhou 510160,China)
出处
《中国当代医药》
2019年第22期15-18,共4页
China Modern Medicine
关键词
高效液相色谱法
聚多卡醇注射液
有关物质
含量
High performance liquid chromatography method
Polidocanol Injection
Related substances
Content
作者简介
杨梅(1986-),女,湖南衡阳人,硕士,主管药师,主要从事化学药品分析检验及标准提高方面的工作.
