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。
Objective To establish the HPLC method for determination of oxysophocarpine （OSC） and optimize the extraction and purification technology of OSC from Sophora alopecuroides by inverse phase membrane. Methods Based on single-factor test, the influence of aqueous phase and organic phase volume ratio, the concentration of sodium hydroxide and hydrochloric acid, and the extraction cycle time were investigated using orthogonal design method. Results OSC was determined by Shim-pack VP-ODS chromatographic column （250 mm ×4.6 mm,5μm）, mobile phase was methanol-0.2% phosphoric acid aqueous solution （7 ： 93）, gradient elution, flow rate was 1 mL/min, column temperature was 30 ℃, and detection wavelength was 221 nm. The ratio of aqueous phase and organic phase volume was 1 ： 1, hydrochloric acid concentration was 0.03 mol/L, sodium hydroxide concentration was 0.5 mol/L, water pump flow rate was 6 mL/min, and cycle time was 60 rain. The extraction rate of OSC 98.21% in 60 rain was under the best experimental conditions. OSC had good linearity relationship within the range of 0.01-0.7 mg/mL, r^2 = 0.997 8, and the respective average recovery rate was 97.47%, RSD = 1.95%. Conclusion This extraction technology is simple operation, with low organic solvent consumption, and can be used for alkaloids extraction.
作者
喀日耶姆.艾海提
米尔扎提.麦麦提
艾尔肯.依不拉音
Kariyemu·AiHAiTi MirzatoMAIMAITI Arkin. IBURAIM(, College of Pharmacy, Xinjiang Medical University, Urumqi 830011, China School of Public Health, Xinjiang Medical University, Urumqi 830011, China Central Laboratory of Xinjiang Medical University, Urumqi 830011, China)
出处
《中草药》
CAS
CSCD
北大核心
2017年第4期686-692,共7页
Chinese Traditional and Herbal Drugs
基金
国家自然科学基金资助项目(21162030)
