摘要
目的:建立专属、快速、简单的测定黄藤素含量的氢核磁共振定量分析方法。方法:以DMSO-d_6为溶剂,马来酸为内标,在测试温度为300 K,脉冲宽度9.54μs,弛豫时间15 s和扫描次数为64次条件下测定氢核磁共振谱,通过比较马来酸定量峰面积(A_r)与黄藤素定量峰面积(A_s),计算黄藤素含量。结果:选择黄藤素δ7.10处和马来酸δ6.26处单峰信号作为定量峰,精密度RSD为0.23%(n=6),重复性RSD为1.2%(n=6),质量比Y(m_s/m_r)与其峰面积比X(A_s/A_r)的线性回归方程为Y=3.782X+0.072(r=0.999 9)。3批黄藤素测得含量分别为86.57%、86.94%和87.01%;测定结果与质量平衡法定值结果基本一致。结论:该方法操作简便,测定结果准确,且与结构鉴定同步完成,适用于黄藤素原料药的质量控制。
Objective： To establish a specific, rapid and simple method for the determination of palmatine by quantitative nuclear magnetic resonance （ qNMR ）. Methods： DMSO-d6 was employed as solvent, and maleic acid as an internal standard. The testing temperature was set at 300 K, pulse width was 9.54 μs, the delay time was 15 s and the number of scanning was 64. Under these conditions, the 1H-NMR data of palmatine was obtained, and then calculate the assay of palmatine by comparing the response signal area of palmatine （ As ） with that of maleic acid （Ar ）. Resluts： Proton signal peaks at 67.10 of palmatine and 86.26 of maleic acid served as quantitative peaks, which showed good separation. The precision RSD was 0.23% （ n=6 ） and the repeatability RSD was 1.2% （ n=6 ）. Linear regression of quantitative peak areas ratio （As/At, X ）of palmatinemaleic acid versus mass ratio （ms/ mr, Y）yielded a correlation coefficient of 0. 999 9 and a regression equation of Y=3.782X＋0.072. The contents of 3 batches of palmatine were 86.83%, 86.94% and 87.01%; the results were generally consistent with that of mass balance methods. Conclusion： This method is easy and simple to handle, and the analysis results are accurate. And the structures could also be identified at the same time. Therefore, qNMR could be used for the quality control of palmatine.
作者
王思寰
郝海军
王广东
王迎春
WANG Si-huan HAO Hai-jun WANG Guang-dong WANG Ying-chun(Shanghai Institute of Pharmaceutical Industry, China State Institute of Pharmaceutical Industry, Instrumental Analysis ＆ Research Center, Shanghai 201203, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第4期654-658,共5页
Chinese Journal of Pharmaceutical Analysis
关键词
黄藤素
巴马汀
掌叶防已碱
季铵型生物碱
黄藤
核磁共振波谱
定量氢谱
定量分析
质量控制
palmatine
Bamating
Zhangyefangjijian
quaternary ammonium alkaloids
Fibraureae Caulis
NMR
quantitative 1H-NMR
quantitative analysis
quality control
