盐酸氨基葡萄糖胶囊含量测定方法比较及其不确定度评价  

Comparison of content determination methods for glucosamine hydrochloride capsules and its uncertainty evaluation

作　　者：张婷 周长明 丁锐 王静 Zhang Ting;Zhou Changming;Ding Rui;Wang Jing(Beijing Institute for Drug Control(Beijing Center for Vaccine Control),NMPA Key Laboratory for Research and Evaluation of Generic Drug,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)

机构地区：[1]北京市药品检验研究院(北京市疫苗检验中心),国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《首都食品与医药》2025年第10期157-160,共4页Capital Food Medicine

摘　　要：目的建立盐酸氨基葡萄糖胶囊含量测定的更优方法,并评定其不确定度。方法对盐酸氨基葡萄糖胶囊含量测定方法进行探索性研究,采用phenomenex NH2色谱柱,流动相:磷酸盐缓冲液-乙腈(25∶75),紫外检测器(195nm),进样量10μL,柱温35℃,流速1.5mL·min^(-1)。参照2020年版《中国药典》四部9101药品质量标准分析方法验证指导原则进行专属性、准确度、精密度、定量限、线性、范围耐用性等考察;与国家标准方法进行比较;同时分析测定HPLC方法的不确定度。结果HPLC法测定盐酸氨基葡萄糖浓度在1.88-11.25mg·mL^(-1)范围内线性关系良好,相关系数r为0.998;定量限为0.188mg·mL^(-1);加标回收率为99.57%-100.65%;精密度RSD为0.88%,重复性RSD为0.72%,溶液在8h内稳定。与国家药品标准紫外分光光度法比较,检测结果存在差异,高效液相色谱法操作过程更加简便快捷。HPLC法含量最终测定结果为(101.00±0.01)%,k=2。结论建立盐酸氨基葡萄糖胶囊含量测定的高效液相色谱法,分辨率更高、重现性更好。同时对该方法进行了不确定度评定,可为该品种的质量控制提供量化评价指标。Objective To establish the optimal method for determining the content of glucosamine hydrochloride capsules and evaluate its uncertainty.Methods An exploratory study was conducted on the content determination method of glucosamine hydrochloride capsules.A phenomenex NH2 chromatography column was used,with a mobile phase consisting of phosphate buffer acetonitrile(25∶75)isocratic elution,a UV detector(195nm),an injection volume of 10μL,acolumn temperature of 35℃,and a flow rate of 1.5mL·min^(-1).Conduct inspections on specificity,accuracy,precision,quantification limit,linearity,range durability,etc.In accordance with the validation guidelines for drug quality standard analysis methods in Part 9101 of the 2020 edition of the Chinese Pharmacopoeia;compare with UV spectrophotometry;simultaneously analyze the uncertainty of the HPLC method.Results The HPLC method showed a good linear relationship between the concentration of glucosamine hydrochloride in the range of 1.88-11.25 mg·mL^(-1),with a correlation coefficient r of 0.998;the quantification limit is 0.188mg·mL^(-1);the recovery rate of spiking is 99.57%to 100.65%;the precision RSD is 0.88%,the repeatability RSD is 0.12%,and the solution is stable within 8 hours.Compared with the national drug standard UV spectrophotometry,there are differences in the detection results,and the operation process of high-performance liquid chromatography is more convenient and fast.The final content determination result of HPLC method is(101.00±0.01)%,k=2.Conclusion Establishingahigh-performanceliquid chromatography method for the determination of glucosamine hydrochloride capsules has higher resolution and better reproducibility.At the same time,the uncertainty of this method has been evaluated,which can provide quantitative evaluation indicators for the quality control of this variety.

关 键 词：盐酸氨基葡萄糖胶囊 含量测定 高效液相色谱法 紫外分光光度法 不确定度 

分 类 号：R927.2[医药卫生—药学]