HPLC法测定注射用特利加压素中有关物质  

Determination of related substances in Terlipressin for injection by HPLC

作　　者：王培 段玺玉 鲁鑫 马冰 覃婷婷 白海娇 韩晓捷 WANG Pei;DUAN Xiyu;LU Xin;MA Bing;QIN Tingting;BAI Haijiao;HAN Xiaojie(Tianjin Institute of Drug Control,Tianjin 300070,China)

机构地区：[1]天津市药品检验研究院,天津300070

出　　处：《现代药物与临床》2024年第10期2537-2542,共6页Drugs & Clinic

基　　金：2023年国家药品抽检项目(国药监药管﹝2023﹞2号)。

摘　　要：目的建立HPLC法测定注射用特利加压素中有关物质。方法采用Agilent Poroshell 120EC-C18色谱柱(150mm×4.6 mm,2.7μm);磷酸二氢钾缓冲液–乙腈(90∶10)为流动相A,磷酸二氢钾缓冲液–乙腈(60∶40)为流动相B,梯度洗脱;检测波长为210 nm;体积流量为0.7 mL/min;进样量为20μL;柱温为35℃。按照主成分对照品外标法计算。结果杂质L、K、G、I、D、H、E、F、Y、P、M、B、T、J、N在0.04~40.8μg/mL线性关系良好;平均回收率分别为99.46%、98.35%、98.24%、99.15%、100.01%、99.34%、99.56%、99.42%、98.79%、98.64%、99.16%、98.22%、99.31%、98.11%、99.38%,RSD值分别为0.98%、1.23%、1.45%、0.85%、1.21%、1.09%、1.16%、0.94%、1.25%、0.79%、1.42%、0.92%、0.88%、1.72%、1.26%。结论建立的方法准确、专属性强,可用于注射用特利加压素中有关物质的质量控制。Objective To establish an HPLC method for determination of substances in Terlipressin for injection.Methods Agilent Poroshell 120EC-C18 column(150 mm×4.6 mm,2.7μm)was used.Mobile phase A was potassium dihydrogen phosphate buffer-acetonitrile(90:10),mobile phase B was potassium dihydrogen phosphate buffer-acetonitrile(60:40),and gradient elution was carried on.Detection wavelength was set at 210 nm,volume flow rate was 0.7 mL/min,and injection volume was 20μL.Column temperature was 35℃.The related substances were calculated using the principal component reference standard external standard method.Results The linear range of impurities L,K,G,I,D,H,E,F,Y,P,M,B,T,J,and N was 0.04—40.80μg/mL.The average recovery was 99.46%,98.35%,98.24%,99.15%,100.01%,99.34%,99.56%,99.42%,98.79%,98.64%,99.16%,98.22%,99.31%,98.11%,and 99.38%,respectively,and the RSD value was 0.98%,1.23%,1.45%,0.85%,1.21%,1.09%,1.16%,0.94%,1.25%,0.79%,1.42%,0.92%,0.88%,1.72%,and 1.26%.Conclusion The established method is accurate and highly specific,and can be used for quality control of related substances in Terlipressin for injection.

关 键 词：注射用特利加压素 有关物质 杂质L 杂质K 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]