双三元二维液质联用法测定醋酸奥曲肽及其制剂中的高分子杂质  

Determination of high molecular weight impurities in Octreotide acetate and its preparationsby Two-dimensional liquid chromatography and mass spectrum

作　　者：李茜[1] 梅芊[1] 仲平[1] 刘英[1] LI Qian;MEI Qian;ZHONG Ping;LIU Ying(Henan Institute for Food and Drug Control,Zhengzhou,Henan,450003 P.R.China)

机构地区：[1]河南省食品药品检验所,河南郑州450003

出　　处：《华西药学杂志》2021年第4期458-462,共5页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用双三元二维液质联用法测定醋酸奥曲肽及其制剂中的高分子杂质。方法采用TSK gel G2000 SWXL色谱柱(300 mm×7.8 mm,5μm),流动相为三氟乙酸-乙腈-水(0.05∶30∶70),流速0.7 mL·min^(-1),柱温25℃,检测波长210 nm。结果0.25~4.95μg·mL^(-1)醋酸奥曲肽与峰面积的线性关系良好;定量限及检测限分别为3.0、1.0 ng。结论所用方法可用于醋酸奥曲肽及其制剂中高分子杂质的质量控制。OBJECTIVE To determine high molecular weight impurities in Octreotide acetate and its preparations by Two-dimensional liquid chromatography and mass spectrum.METHODS A TSK gel G2000SWXL column(300 mm×7.8 mm,5μm)was used,with the mobile phase of trifluoroacetic acid-acetonitrile-water(0.05∶30∶70).The flow was 0.7mL·min^(-1)with the column temperature of 25℃ and the detection wavelength of 210 nm.RESULTS The linear ranges of octreotide acetate was 0.25-4.95μg·mL^(-1),the quantitation limit was 3.0 ng and the detection limit was 1.0 ng.CONCLUSION This method is suitable for the quality control of high molecular weight impurities in Octreotide acetate and its preparations.

关 键 词：醋酸奥曲肽 高分子杂质 醋酸奥曲肽二聚体 质量控制 双三元二维液相色谱 质谱 

分 类 号：R917[医药卫生—药物分析学]