碳酸钙甘氨酸胶囊/甘氨酸碳酸钙胶囊溶出度检查及含量测定  

Determination of Dissolution and Content Determination of Calcium Carbonate and Glycine in Calcium Carbonate and Glycine Capsules/Glycine and Calcium Carbonate Capsules

作　　者：李梓莹 LI Ziying(Guangzhou Institute for Drug Control,Guangzhou,Guangdong 510160,China)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《今日药学》2023年第9期694-699,共6页Pharmacy Today

基　　金：国家药典委员会标准修订研究课题(2019H016)。

摘　　要：目的建立容量法和高效液相色谱法测定碳酸钙甘氨酸胶囊/甘氨酸碳酸钙胶囊中碳酸钙与甘氨酸的溶出量及含量测定方法。方法(1)碳酸钙测定:采用容量法,用乙二胺四醋酸二钠滴定液滴定至溶液显纯蓝色。(2)甘氨酸测定:氨基键合硅胶色谱柱,以乙腈-0.05 mol·L^(-1)磷酸二氢钾溶液(68∶32)为流动相,检测波长205 nm,进样20μL(含量测定进样10μL),以外标法计算甘氨酸溶出量及含量。结果甘氨酸在5~150μg·mL^(-1)范围内线性关系良好r=0.9998(n=8),供试品溶液在15 h内稳定,辅料无干扰。甘氨酸在0.05~2.00 mg·mL^(-1)范围内线性关系良好r=1(n=7),定量限为4.2943μg·mL^(-1),检测限为1.2883μg·mL^(-1)。供试品溶液在15 h内稳定,辅料无干扰。结论建立的方法测定碳酸钙甘氨酸胶囊/甘氨酸碳酸钙胶囊中碳酸钙与甘氨酸的溶出量及含量简便快捷,能准确测定。OBJECTIVE To develop volumetric method and HPLC method to determine the dissolution and content determination of calcium carbonate and glycine capsules/glycine and calcium carbonate capsules.METHODS(1)Calcium carbonate:volumetric method.The solution was titrated with disodium edetate titrant until the solution showed pure blue.(2)Glycine:the determination was performed on amino-bonded silica gel chromatographic(ChromCore NH_(2),4.6 mm×250 mm,5μm)column,with acetonitrile-0.05 mol·L^(-1)potassium dihydrogen phosphate(68∶32)as the mobile phase.The detection wavelength was 205 nm.The injection volume was 20μL(content determination injection volume was 10μL).The glycine were quantified by external standard method.RESULTS Dissolution:glycinehad a good linear relationship in the range of 5-150μg·mL^(-1)(n=8,r=0.9998).The test solution was stable in 15 hours with non-interference of auxiliary materials.And content determination:glycinehad a good linear relationship in the range of 0.05-2.00 mg·mL^(-1)(n=7,r=1).The limit of quantification was 4.2943μg·mL^(-1),the limit of detection was 1.2883μg·mL^(-1).The test solution was stable in 15 hours,and the auxiliary materials were noninterference.CONCLUSION The method is convenient,quick and accurate,and can be applied to the dissolution and content determination in calcium carbonate and glycine capsules and glycine and calcium carbonate capsules.

关 键 词：碳酸钙 甘氨酸 容量法 高效液相色谱法 溶出度 含量测定 

分 类 号：R917[医药卫生—药物分析学]