基于特征肽的超高效液相色谱-串联质谱法测定复方胃蛋白酶颗粒的溶出度  

Dissolution Determination of Compound Saccarated Pepsin Granules with Marker Peptide based on UPLC-MS/MS

作　　者：杭宝建 巩丽萍 陈晓 咸瑞卿 石峰 HANG Bao-jian;GONG Li-ping;CHEN Xiao;XIAN Rui-qing;SHI Feng(Shandong Research Center of Engineer and Technology for Consistency Evaluation of Generic Drugs,National Medical Products Administration(NMPA)Key laboratory for Quality Evaluation of Gelatin Products,Shandong Institute for Food and Drug Control,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院国家药品监督管理局仿制药研究与评价重点实验室山东省仿制药一致性评价工程技术研究中心,山东济南250101

出　　处：《化学试剂》2021年第7期941-944,共4页Chemical Reagents

基　　金：国家药品评价性抽验计划项目(食药监办药化监[2017]15号)。

摘　　要：建立以特征肽为指标的自身对照法测定复方胃蛋白酶颗粒中胃蛋白酶溶出度的方法。选择多肽GTIGIGTPAQDF作为胃蛋白酶的特征肽,建立超高效液相色谱-串联质谱多反应监测测定胃蛋白酶含量的方法。以水作为溶出介质,浆法,转速为50 r/min,采用自身对照法计算溶出度。特征肽在0.010 5~0.525μg/mL内线性关系良好(R2=0.998),精密度和重复性均良好,回收率101.2%。7个厂家产品的溶出度均大于80%,溶出度相似度f2因子值除1家企业外均大于50%,溶出行为基本相似。方法准确、可靠,可用于测定该制剂的溶出度。We established the self-control method for the determination of dissolution of pepsin in compound saccarated pepsin granules with marker peptide.Pepsin was quantified by its marker peptide GTIGIGTPAQDF using LC-MS/MS technique in multiple reaction monitoring mode.Paddle method was adopted with water as the dissolution medium.The rotation speed was 50 r/min.The dissolution was calculated by using self-control method.The linear range of marker peptide concentration was 0.010 5~0.525 μg/mL(R2=0.998).The method has good precision and reproducibility.The average recovery was 101.2%.The dissolution of the samples from seven manufacturers was all greater than 80%,and the f2 factor value was all greater than 50% except for one manufacturer, and the dissolving behavior is basically similar.The method is accurate, reliable and can be used for determining the dissolution of the preparation.

关 键 词：复方胃蛋白酶颗粒 特征肽 超高效液相色谱-串联质谱 自身对照法 溶出度 

分 类 号：R917[医药卫生—药物分析学]