【摘要】：目的建立氧化槐果堿(OSC)的HPLC測定方法及苦豆子中OSC的逆三相膜循環(huán)萃取分離工藝。方法在單因素試驗的基礎上,采用正交試驗考察水相和有機相(氯仿)體積比、鹽酸濃度、氫氧化鈉濃度和提取時間對OSC提取工藝的影響,確定最佳提取工藝。結果 HPLC測定條件:Shim-pack VP-ODS色譜柱(250 mm×4.6 mm,5μm),流動相為甲醇-0.2%磷酸水溶液(7∶93),梯度洗脫,體積流量1 m L/min,進樣量5μL,柱溫30℃,檢測波長221 nm,OSC在0.01~0.7 mg/m L時線性關系良好,r~2=0.997 8,平均回收率為97.47%,RSD為1.95%。萃取純化工藝參數(shù):水相和有機相體積比為1∶1,鹽酸濃度為0.3 mol/L,氫氧化鈉濃度為0.75 mol/L,循環(huán)泵體積流量6 m L/min,循環(huán)時間60 min;最佳條件下OSC溶液在60 min內萃取率達到98.21%。結論該提取工藝操作簡單,有機溶劑消耗量低,可用于生物堿的萃取。
[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，

本文編號：2309241