生长抑素及制剂中多聚体的定量研究  

Quantitative study on polymer in somatostatin and preparation

作　　者：张伟[1] 张慧[1] 梁成罡[1] ZHANG Wei;ZHANG Hui;LIANG Chenggang(Division of Hormone,National Institutes for Food and Drug Control,NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院激素室,国家药品监督管理局化学药品质量研究与评价重点实验室,北京102629

出　　处：《中国药品标准》2023年第6期596-600,共5页Drug Standards of China

基　　金：国家药典委员会药品标准制修订研究课题(2020H012)。

摘　　要：目的:建立高效液相色谱-分子排阻色谱法(HPLC-SEC)测定生长抑素及制剂中的多聚体,并进行了方法学验证。方法:采用TSKgel G2000SWXL色谱柱(7.8 mm×300 mm,5μm),流动相为乙腈-水-三氟乙酸(20∶80∶0.1,体积比),线性等度洗脱,流速0.5 mL·min^(-1),柱温25℃,进样量为100μL;紫外检测器,检测波长为215 nm;标准曲线法和面积归一化法计算多聚体含量。结果:生长抑素二聚体的检测限为5.2 ng,定量限为15.6 ng,线性范围为0.1~5μg·mL^(-1)(r=0.999 6),平均回收率(n=3)为100.3%(RSD=0.52%)。结论:该方法快速、灵敏、准确,能够对生长抑素及制剂中的多聚体进行质控。Objective:An HPLC-SEC method for the determination of polymer in somatostatin and preparation was established and validated.Methods:TSKgel G2000SWXL column(7.8 mm×300 mm,5 μm) was used.The mobile phase consisted of acetonitrile-water-trifluoroacetic acid(20∶80∶0.1,volume ratios) at the flow rate of 0.5 mL·min~(-1).The column temperature was set at 25 ℃,and the sampling volume was 100 μL.Detection wavelength was 215 nm.Polymeric content was calculated by standard curve method and area normalization method.Results:The detection limit and quantitation limit of dimer were 5.2 ng and 15.6 ng,respectively.The linear range was 0.1-5 μg·mL~(-1)(r=0.999 6).The average recovery(n=3) was 100.3%(RSD=0.52%).Conclusions:This method is rapid,sensitive and accurate,and can be used to control the quality of polymer in somatostatin and preparation.

关 键 词：高效液相色谱-分子排阻色谱法 紫外 生长抑素 制剂 多聚体 

分 类 号：R921.2[医药卫生—药学]