注射用生长抑素中有关物质检查方法研究  

Detection Method of Related Substances in Somatostatin for Injection

作　　者：刘冰滢 薛巧如[1] 彭诗斯 陈华[1] 穆矛 LIU Bingying;XUE Qiaoru;PENG Shisi;CHEN Hua;MU Mao(Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《中国药学杂志》2024年第13期1252-1261,共10页Chinese Pharmaceutical Journal

基　　金：广东省医学科学技术研究基金资助(B2021404);广东省药品监督管理局科技创新项目资助(2022TDZ203,2022TDB02);广东省药品检验所所内项目资助(SN2022022)。

摘　　要：目的建立注射用生长抑素中有关物质的高效液相色谱检测方法。方法色谱柱为C18柱;以磷酸二氢钾溶液-乙腈为流动相,梯度洗脱。检测波长为215 nm,柱温为50℃。结果本研究新建方法能够将主成分以及7种主要降解杂质有效分离,生长抑素和7种杂质峰面积与浓度线性关系良好(r≥0.9991,n=8);7种杂质精密度、稳定性、重复性试验的相对标准偏差(RSD)均低于3.6%;平均回收率在100.0%~104.4%之间(n=9)。应用本研究新建方法测得样品中的杂质含量高于《欧洲药典》和《中国药典》方法所测得结果。结论该方法操作简便,结果准确,重复性好,可对注射用生长抑素杂质进行质量控制,并为该品种的标准修订提供方法依据。OBJECTIVE To establish a high performance liquid chromatography(HPLC)method for the detection of related substances in somatostatin for injection.METHODS The determination was performed on a C18 column with mobile phases consisting of potassium dihydrogen phosphate solution and acetonitrile by gradient elution.The detection wavelength was set at 215 nm and the column temperature was maintained at 50℃.RESULTS The established method can effectively separate the main components and seven major degradation impurities.The peak area of somatostatin and 7 kinds of impurities had good linear relationships with the concentration(r≥0.9991,n=8).Relative standard deviation(RSD)of precision,stability and repeatability tests of 7 kinds of impurities were all lower than 3.6%.The average recoveries of 7 kinds of impurities ranged from 100.0%to 104.4%(n=9).The impurity content determined by the established method is higher than that determined by the European Pharmacopoeia(EP)and Chinese Pharmacopoeia(Ch.P).CONCLUSION The method is simple,accurate and stable.It can control the impurities in somatostatin for injection and provide a basis for improving the standard of this drug.

关 键 词：注射用生长抑素 高效液相色谱法 有关物质 方法学验证 方法比较 

分 类 号：R917[医药卫生—药物分析学]