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目的:建立高纯度栀子苷的工业色谱分离工艺。方法:采用D-101型大孔吸附树脂对栀子水提液中栀子苷进行富集,经工业色谱精制纯化,分别运用TLC,HPLC和电喷雾质谱(ESI-MS)对栀子苷进行含量测定和表征。HPLC条件为流动相乙腈-水(15∶85),检测波长237 nm;ESI-MS条件为干燥气温度350℃,毛细管电压4 000 V,分离器电压65 V,传输电压135 V,质荷比扫描范围50~1 300,正离子模式,流动相甲醇-水(1∶1),流速0.5 mL·min-1,不经过色谱柱。结果:栀子苷的最佳纯化工艺为加3 BV水洗脱,弃去水洗液,继用30%乙醇2.5 BV洗脱,收集洗脱液,加乙酸乙酯-甲醇(10∶1)混合液以300 mL·min-1的流速进行洗脱,TLC跟踪检测,洗脱液减压浓缩至出现大量白色固体,抽滤,干燥;栀子苷纯度达98.6%,转移率68.9%。结论:采用动态轴向工业色谱制备栀子苷的工艺稳定可靠、重复性好且适合工业化大生产。
Objective: To establish a high-purity geniposide industrial chromatographic separation process. Methods: Geniposide in Gardenia water extract was concentrated by D-101 macroporous resin and purified by industrial chromatography. Geniposide was purified by TLC, HPLC and ESI-MS respectively Determination and characterization. The conditions of HPLC were acetonitrile-water (15:85) and detection wavelength of 237 nm. The conditions of ESI-MS were dry gas temperature 350 ℃, capillary voltage 4 000 V, separator voltage 65 V, transmission voltage 135 V, Scanning range 50 ~ 1 300, positive ion mode, mobile phase methanol-water (1: 1), flow rate 0.5 mL · min-1, without passing through the column. Results: The best purification technology of geniposide was to add 3 BV water, discard the washing solution and elute with 30% ethanol 2.5 BV. Eluate was collected and mixed with ethyl acetate - methanol (10: 1) The solution was eluted at a flow rate of 300 mL · min-1 and monitored by TLC. The eluate was concentrated under reduced pressure to a large amount of white solid, which was suction-filtered and dried. The purity of geniposide reached 98.6% with a transfer rate of 68.9%. Conclusion: The process of preparation of geniposide by dynamic axial industrial chromatography is stable and reliable, reproducible and suitable for industrialized large-scale production.