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| NMR测定丹酚酸B标准品中有机溶剂残留 |
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许磊1,2, 王萌1, 王跃飞1, 姜苗苗1
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1.天津中医药大学, 天津市现代中药重点实验室, 天津 300193;2.天津国际生物医药联合研究院, 中药新药研发中心, 天津 300457
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| 摘要: |
| [目的] 用定量核磁共振(QNMR)技术建立中药来源的标准品化合物丹酚酸B中残留甲醇、乙醇和乙酸含量的快速分析方法。[方法] 采用BRUKER AVANCEⅢ 600型超导核磁共振波谱仪采集谱图, 观频率600.23 MHz,测定温度298 K.谱宽12 019.2 Hz,采样数据点65 536,扫描次数16次, 延迟时间15 s.[结果] 所有标准曲线在1.22~2 430 mg/L范围内线性良好(r2>0.999 5),平均回收率(n=6)在 105%~109%之间。[结论] 本方法快速、准确, 可应用于样品有机溶剂残留的检测。 |
| 关键词: 液体核磁共振 有机溶剂残留 丹酚酸B 定量分析 |
| DOI：10.11656/j.issn.1672-1519.2015.08.15 |
| 分类号: |
| 基金项目:国家自然科学基金项目(81303181). |
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| Determination of the residual organic solvents in Salvianolic acid B by NMR |
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XU Lei1,2, WANG Meng1, WANG Yue-fei1, JIANG Miao-miao1
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1.Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China;2.Research and Development Center of Traditional Chinese Medicine, Tianjin International Joint Academy of Biotechnology and Medicine, Tianjin 300457, China
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| Abstract: |
| [Objective] To establish an QNMR method for the determination of methanol, ethanol and acetic acid in Salvianolic acid B. [Methods] The 1H-NMR spectra was performed on a Bruker AV Ⅲ 600 MHz NMR spectrometer with a proton frequency of 600.23 MHz and a temperature of 298 K. [Results] Each experiment consisted of 16 scans with a spectral width of 12 019.2 Hz and a recycle delay of 15 s per scan. All the calibration curves showed good linearity (r2>0.999 5) in the range of 1.22~2 430 mg/L. The average recoveries were 105%~109%(n=6). [Conclusion] The method is rapid and accurate, which is helpful for the determination of the residua1 organic solvents in Salvianolic acid B. |
| Key words: liquid NMR residua1 organic solvent Salvianolic acid B quantitative analysis |
