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目的建立氧化槐果碱(OSC)的HPLC测定方法及苦豆子中OSC的逆三相膜循环萃取分离工艺。方法在单因素试验的基础上,采用正交试验考察水相和有机相(氯仿)体积比、盐酸浓度、氢氧化钠浓度和提取时间对OSC提取工艺的影响,确定最佳提取工艺。结果 HPLC测定条件:Shim-pack VP-ODS色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%磷酸水溶液(7∶93),梯度洗脱,体积流量1 m L/min,进样量5μL,柱温30℃,检测波长221 nm,OSC在0.01~0.7 mg/m L时线性关系良好,r~2=0.997 8,平均回收率为97.47%,RSD为1.95%。萃取纯化工艺参数:水相和有机相体积比为1∶1,盐酸浓度为0.3 mol/L,氢氧化钠浓度为0.75 mol/L,循环泵体积流量6 m L/min,循环时间60 min;最佳条件下OSC溶液在60 min内萃取率达到98.21%。结论该提取工艺操作简单,有机溶剂消耗量低,可用于生物碱的萃取。
OBJECTIVE To establish an HPLC method for the determination of oxysophthalidine (OSC) and reverse phase three-phase membrane (CCS) cyclic extraction and separation of OSC in Sophora alopecuroides. Methods Based on the single factor experiment, orthogonal experiment was used to investigate the influence of the volume ratio of the aqueous phase to the organic phase (chloroform), the concentration of hydrochloric acid, the concentration of sodium hydroxide and the extraction time on the extraction process of OSC, and the optimum extraction process was determined. Results The HPLC conditions were as follows: Shim-pack VP-ODS column (250 mm × 4.6 mm, 5 μm) with methanol-0.2% phosphoric acid solution (7:93), gradient elution at a flow rate of 1 mL / The injection volume was 5μL, the column temperature was 30 ℃, the detection wavelength was 221 nm, and the OSC was good at 0.01-0.7 mg / mL. The average recovery was 97.47% and RSD was 1.95%. Extraction and purification process parameters: the volume ratio of aqueous phase to organic phase was 1: 1, the concentration of hydrochloric acid was 0.3 mol / L, the concentration of sodium hydroxide was 0.75 mol / L, the circulation pump volume flow rate was 6 m L / min and the cycle time was 60 min. Under the optimum conditions, the extraction rate of OSC solution reached 98.21% within 60 min. Conclusion The extraction process is simple, low consumption of organic solvents, alkaloids can be used for extraction.