Optimization of the separation and purification process for iridoid glycosides from Lamioplomisrotata
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摘要: 目的 优化独一味总环烯醚萜苷的制备工艺，获取纯度相对较高的总环烯醚萜苷。 方法 以甲醇-水为流动相，梯度洗脱方式建立分离分析独一味总环烯醚萜苷的高效液相色谱方法，实现各组分的最佳分离，统计、记录其三维吸收图谱，并结合紫外全波长扫描，对前期制备的独一味总环烯醚萜苷中影响纯度的杂质特征进行分析，根据杂质特性优化大孔树脂结合聚酰胺柱制备过程，紫外实时监测，剔除杂质，产品溶液经冷冻干燥获得冻干粉，并以HPLC对比前后制备工艺产品成分差异。 结果 工艺优化前产品中环烯醚萜苷含量为69.06%，优化后含量为90.60%，含量提升21.54%；本次制备总产率为16.70%（以水提取物的质量为参照），总环烯醚萜苷转移率为74.72%（相对于水提取物中总环烯醚萜苷的质量）。 结论 优化过程简单，操作步骤可控，易于实现，纯化效果显著。Abstract: Objective To obtain iridoid glycosides with relatively high purity by the optimization of the preparation process of iridoid glycosides from Lamioplomisrotata. Methods Used methanol-water mobile phase with gradient run to set up an HPLC method and achieved the best separation of each composition. Recorded and calculated statistics for its three-dimensional absorption spectrum combined with UV visible wavelength scanning to analyze the characteristics of the impurities, which have affected the purity of previous preparations of iridoid glycosides from Lamioplomisrotata. To optimize the process, a macroporous adsorptive resin chromatographic column and a polyamide chromatographic column were used on the basis of characteristics of the impurities. A real time UV visible wavelength scan was applied to monitor the effluent components of each column to remove the impurities. Merged the ethanol elution which had the characteristic absorption at 235 nm and smaller absorptions at other wavelengths. The target solutions were cryodesiccated. Compared the differences of the iridoid glycoside compositions at equal concentrations before and after the experiment by HPLC. Results The contents of iridoid glycosides from Lamioplomisrotata before and after the purification process were 69.06% and 90.60% respectively. The yield was 16.70% (use the quality of the water extract as a reference).The transfer rate of iridoid glycosides was 74.72% (relative to the quality of water extract of total iridoid glycosides). Compared with the previous preparation technology, the content was increased to 21.54%. Conclusion The optimization process was simple and practicable with high efficiency, which made a significant improvement in the purity of the iridoid glycosides from Lamioplomisrotata.
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Key words:
- Lamiophlomisrotata (Benth.) /
- iridoids glycosides /
- preparation /
- process optimization /
- content
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