苦豆子中氧化槐果碱的逆三相膜循环萃取分离
发布时间：2018-11-04 08:09
【摘要】：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。
[Abstract]:Objective to establish a HPLC method for the determination of oxysophorine (OSC) and an inverse three-phase membrane cyclic extraction process for the separation of OSC from Sophora flavescens. Methods on the basis of single factor experiment, the effects of volume ratio of aqueous phase and organic phase (chloroform), concentration of hydrochloric acid, concentration of sodium hydroxide and extraction time on the extraction process of OSC were investigated by orthogonal test. Results HPLC determination conditions were as follows: Shim-pack VP-ODS column (250 mm 脳 4.6 mm,5 渭 m),) as mobile phase, methanol-0.2% phosphoric acid solution (7:93), gradient elution, volume flow rate of 1 mL / min, injection volume of 5 渭 L, column temperature of 30 鈩，
本文编号：2309241
[Abstract]:Objective to establish a HPLC method for the determination of oxysophorine (OSC) and an inverse three-phase membrane cyclic extraction process for the separation of OSC from Sophora flavescens. Methods on the basis of single factor experiment, the effects of volume ratio of aqueous phase and organic phase (chloroform), concentration of hydrochloric acid, concentration of sodium hydroxide and extraction time on the extraction process of OSC were investigated by orthogonal test. Results HPLC determination conditions were as follows: Shim-pack VP-ODS column (250 mm 脳 4.6 mm,5 渭 m),) as mobile phase, methanol-0.2% phosphoric acid solution (7:93), gradient elution, volume flow rate of 1 mL / min, injection volume of 5 渭 L, column temperature of 30 鈩，
本文编号：2309241
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