| 引用本文: | 晏堂,楼丽,张苏霞,余丽双,刘永静.杜鹃素对映体的分离及其在中药材中的含量测定[J].中国现代应用药学,2024,41(1):80-87. |
| YAN Tang,LOU Li,ZHANG Suxia,YU Lishuang,LIU Yongjing.Separation of Farrerol Enantiomers and Its Content Determination in Chinese Materia Medica[J].Chin J Mod Appl Pharm(中国现代应用药学),2024,41(1):80-87. |
|
| 摘要: |
| 目的 建立杜鹃素对映体分离的HPLC方法，并应用于满山红和照山白药材中的对映体含量测定。方法 用HPLC对杜鹃素对映体进行拆分，优化手性柱种类、流动相比例、流速和柱温的色谱条件。对手性热力学拆分进行探讨，计算杜鹃素对映体在色谱柱分离的焓变、熵变、焓变差值和熵变差值等热力学参数。并在最佳分离条件测定了满山红和照山白2种药材中2个对映体的含量。结果 确定了杜鹃素的2个对映体的最佳分离条件：色谱柱为Chiralcel OJ-RH(4.6 mm×150 mm，5 μm)，乙腈-水(40∶60)为流动相等度洗脱，流速为0.5 mL·min–1，柱温为25 ℃，检测波长为295 nm。在最佳分离条件下，杜鹃素对映体的分离度达到1.5，表明杜鹃素的2个对映体能够完全分离。当柱温为20~35 ℃时，分离因子随着温度的升高呈降低趋势，2个对映体的lnα与1/T呈良好的线性关系，手性拆分过程受焓的控制。将所建立的杜鹃素对映体分离方法应用于中药材满山红、照山白中的杜鹃素对映体含量测定，杜鹃素的2个对映体线性范围分别为0.718~57.44 μg·mL–1和1.28~102.24 μg·mL–1，在3个批次的满山红中杜鹃素的2个对映体的平均含量分别为0.228 2和0.466 2 mg·g–1；3个批次的照山白中杜鹃素的2个对映体的平均含量分别为0.416 8和0.707 3 mg·g–1。结论 该方法简便高效，适用于中药中杜鹃素对映体的含量测定。 |
| 关键词: 杜鹃素 对映体；高效液相色谱法 满山红 照山白 含量测定 手性分离 |
| DOI：10.13748/j.cnki.issn1007-7693.20224177 |
| 分类号:R284.1 |
| 基金项目: |
|
| Separation of Farrerol Enantiomers and Its Content Determination in Chinese Materia Medica |
|
YAN Tang, LOU Li, ZHANG Suxia, YU Lishuang, LIU Yongjing
|
|
School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350000, China
|
| Abstract: |
| OBJECTIVE To establish an HPLC method for the separation of enantiomers of farrerol, and apply it to the determination of the content of enantiomers in Rhododendri Daurici Folium and Rhododendron Micranthum. METHODS HPLC was used to separate the farrerol enantiomers, and the chromatographic conditions of chiral column type, mobile phase ratio, flow rate, and column temperature were optimized. The thermodynamic separation of farrerol enantiomers was discussed. Thermodynamic parameters such as enthalpy change, entropy change, enthalpy change and entropy change were calculated. And the contents of two enantiomers in Rhododendri Daurici Folium and Rhododendron Micranthum were determined under the optimum resolution conditions. RESULTS The optimum separation conditions for two enantiomers of farrerol were determined as follows: Chiralcel OJ-RH(4.6 mm×150 mm, 5 μm), equilibrium elution of acetonitrile-water(40∶60), the flow rate of 0.5 mL·min–1, the column temperature of 25 ℃, and the detection wavelength of 295 nm. Under the optimum separation conditions, the resolution of farrerol enantiomers reached 1.5, indicating that the two enantiomers of the farrerol could be completely separated. When the column temperature was between 20 ℃ and 35 ℃, the separation factor decreased with the increase of temperature. The lnα of the two enantiomers of farrerol showed a good linear relationship with 1/T, and the chiral reselution process was controlled by enthalpy. The enantiomer separation method of farrerol was applied to the determination of farrerol enantiomer in Chinese medicinal materials of Rhododendri Daurici Folium and Rhododendron Micranthum. The linear relationship between the two enantiomers of farrerol were good in the range of 0.718–57.44 μg·mL–1 and 1.28–102.24 μg·mL–1, respectively. And the contents of the two enantiomers of farrerol in Rhododendri Daurici Folium were 0.228 2 and 0.466 2 mg·g–1, respectively. And the contents of the two enantiomers of farrerol in Rhododendron Micranthum were 0.416 8 and 0.707 3 mg·g–1, respectively. CONCLUSION This method is simple, efficient and suitable for the determination of farrerol enantiomers in traditional Chinese medicine. |
| Key words: farrerol enantiomers HPLC Rhododendri Daurici Folium Rhododendron Micranthum content determination chiral resolution |
