核磁共振波谱法测定片剂中盐酸巴马汀含量
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摘要
以氘代甲醇为溶剂,马来酸为内标,通过比较马来酸内标峰与盐酸巴马汀定量峰的峰面积,采用核磁共振法测定了黄藤素片中盐酸巴马汀的含量。结果显示,该方法的线性范围为1. 00～10. 00 g/L,相关系数(r)为0. 999 3,定量下限为25. 0 mg/L,检出限为8. 5 mg/L,回收率为98. 5%～104%。测定结果与高效液相色谱法基本一致。该方法操作简便、测定结果准确,且与结构鉴定同步完成,适用于黄藤素片的质量控制。
A method of proton nuclear magnetic resonance was developed for the determination of hydrochloride palmatinein in tablets. CD3 OD was employed as solvent and maleic acid as an internal standard,the1 H NMR spectra were obtained with a Bruker AVANCE Ⅲ 400 spectrometer. The content of hydrochloride palmatinein in tablets was determined by comparing the response signal areas of the internal standard( maleic acid,Ar) and hydrochloride palmatine( As). Results showed that there was a linear relationship for hydrochloride palmatine in the range of 1. 00-10. 00 g/L with its correlation coefficient of 0. 999 3. The limit of quantitation( LOQ) was 25. 0 mg/L and the limit of detection( LOD) was 8. 5 mg/L. The recoveries were in the range of 98. 5%-104%. The content of hydrochloride bamatine in tablets was determined by high performance liquid chromatography( HPLC) and proton nuclear magnetic resonance( qNMR),respectively. Results indicated that the two methods had no difference. The qNMR method was easy and simple to handle,and the analysis results was accurate. Furthermore,the structure of the analyte could be identified at the same time. Therefore,q NMR could be used for the quality control of Huangtengsu tablet.
A method of proton nuclear magnetic resonance was developed for the determination of hydrochloride palmatinein in tablets. CD3 OD was employed as solvent and maleic acid as an internal standard,the1 H NMR spectra were obtained with a Bruker AVANCE Ⅲ 400 spectrometer. The content of hydrochloride palmatinein in tablets was determined by comparing the response signal areas of the internal standard( maleic acid,Ar) and hydrochloride palmatine( As). Results showed that there was a linear relationship for hydrochloride palmatine in the range of 1. 00-10. 00 g/L with its correlation coefficient of 0. 999 3. The limit of quantitation( LOQ) was 25. 0 mg/L and the limit of detection( LOD) was 8. 5 mg/L. The recoveries were in the range of 98. 5%-104%. The content of hydrochloride bamatine in tablets was determined by high performance liquid chromatography( HPLC) and proton nuclear magnetic resonance( qNMR),respectively. Results indicated that the two methods had no difference. The qNMR method was easy and simple to handle,and the analysis results was accurate. Furthermore,the structure of the analyte could be identified at the same time. Therefore,q NMR could be used for the quality control of Huangtengsu tablet.
引文
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[3] Guo L C,Hao H J,Du L Y. J. Instrum. Anal.(郭留城,郝海军,杜利月.分析测试学报),2018,37(4):492-495.
[4] Hao H J,Jia Y Z,Han R,Hu B. Chin. J. Pharm.(郝海军,贾幼智,韩茹,胡彬.中国医药工业杂志),2017,48(5):711-714.
[5] Wang S H,Hao H J,Jiang C N,Wang G D,Wang Y C. Central South Pharm.(王思寰,郝海军,江茶农,王广东,王迎春.中南药学),2017,15(2):214-217.
[6] Li C X,Wang X P,Cui F,Hao H J. Herald Med.(李承欣,王雪萍,崔锋,郝海军.医药导报),2017,36(12):1398-1401.
[7] Chinese Pharmacopoeia Commission. Chinese Pharmacopoeia:PartⅠ. Beijing:China Medical Science Press(国家药典委员会.中国药典:一部.北京:中国医药科技出版社),2015:1481.
[8] Zhang H Y,Zhang S,Xia H X,Cai C T,Rao G X. J. Yunnan Univ. Tradit. Chin. Med.(张慧颖,张森,夏海星,蔡传涛,饶高雄.云南中医学院学报),2008,31(4):9-12.
[9] Wang S H,Hao H J,Wang G D,Wang Y C. Chin. J. Pharm. Anal.(王思寰,郝海军,王广东,王迎春.药物分析杂志),2017,37(4):654-658.
[10] Chia Y L,Hong X X,Quan B H,Tian S W. J. Chromatogr. A,2009,1216(11):2124-2129.