药用辅料氧化镁中氧化钙测定方法的改进  

Improvement of determination method of calcium oxide inmagnesium oxide of pharmaceutical excipients

作　　者：伍伟聪[1] 郭雅娟 王淼[1] 王彩媚[1] WU Weicong;GUO Yajuan;WANG Miao;WANG Caimei(Guangdong Institute for Drug Control,NMPA Key Laboratory of Quality Control and Evaluation of Pharmaceutical Excipints,Guangdong 510663,China)

机构地区：[1]广东省药品检验所,国家药品监督管理局药用辅料质量控制与评价重点实验室,广州510663

出　　处：《中国药品标准》2022年第5期486-489,共4页Drug Standards of China

基　　金：国家药品标准提高研究课题(编号:2019Y034)。

摘　　要：目的:建立火焰原子吸收光谱法测定药用辅料氧化镁中氧化钙的量,对《中国药典》2020年版四部中氧化镁与轻质氧化镁的氧化钙测定方法进行了完善。方法:在盐酸溶液介质中,采用火焰原子化器,钙-空心阴极灯(Heraeus),检测波长:422.7 nm,狭缝宽度:0.5 nm,灯电流:10 mA,火焰类型:空气-乙炔。对所建方法进行了方法学考察,并与滴定法结果进行比较。结果:在0~15μg·mL^(-1)浓度范围内,钙离子的线性关系良好(r=0.9988,n=4),精密度RSD为0.9%(n=6),重复性RSD为2.2%(n=6),平均回收率为94.3%。测定19批样品中氧化钙,结果均小于0.8%。AAS法测定结果均高于滴定法结果。结论:经方法验证与结果比较分析,本方法准确性高,可满足药用辅料氧化镁中氧化钙的测定。建议《中国药典》2020年版第一增补本氧化钙的限度修订为不得过1.5%。Objective:To establish the method of flame atomic absorption spectrometry for determination of calcium oxide in pharmaceutical excipient magnesium oxide,and improve the determination method of calcium oxide for magnesium oxide and light magnesium oxide in the Chinese Pharmacopoeia 2020 VolⅣ.Methods:In the hydrochloric acid solution medium,a flame atomizer,calcium-hollow cathode lamp(Heraeus),detection wavelength:422.7 nm,slit width:0.5 nm,lamp current:10 mA,flame type:air-acetylene.A methodological investigation of the established method was carried out and compared with the results of the titration method.Results:In the concentration range of 0-15μg·mL^(-1),the linearity of calcium ions was good(r=0.9988,n=4),the precision RSD was 0.9%(n=6),and the repeatability RSD was 2.2%(n=6),and the average recovery was 94.3%.Calcium oxide in 19 batches of samples was determined,and the results were all less than 0.8%.The results of AAS method were higher than those of titration method.Conclusion:After method validation and result comparison analysis,this method has high accuracy and can satisfy the determination of calcium oxide in magnesium oxide as a pharmaceutical excipient.It is suggested that the limit of calcium oxide in the first supplement of the Chinese Pharmacopoeia 2020 should be revised to no more than 1.5%.

关 键 词：药用辅料 氧化镁 氧化钙 火焰原子吸收光谱法 滴定法 

分 类 号：R921.2[医药卫生—药学]