大孔吸附树脂纯化雷公藤4种有效成分的工艺研究Δ

摘要

目的：研究大孔吸附树脂纯化雷公藤药材中4种有效成分的工艺。方法：通过静态吸附及解吸试验，以雷公藤内酯醇、雷公藤内酯甲、雷公藤内酯酮、雷公藤红素的吸附率和解吸率为指标，考察9种型号大孔吸附树脂（ADS-5、ADS-8、HPD100、HPD300、HPD400、HPD450、HPD700、HPD722及HPD750）对雷公藤4种有效成分的纯化性能，筛选最优大孔树脂；以有效成分转移率为考察指标，采用单因素试验考察不同上样方法、拌样树脂占树脂总量比例、树脂-药材质量比、清洗液（种类、用量及清洗流速）、树脂径高比、洗脱液（体积、流速）对吸附的影响，确定最优的洗脱工艺参数条件并进行验证试验。结果：确定HPD722树脂为吸附树脂；树脂径高比为1∶10，树脂-药材质量比为1∶2，拌样树脂占树脂总量比例为1∶10，湿法装柱，拌树脂上样；用12 BV的20％乙醇以12 BV/h的流速清洗，后用12 BV的95％乙醇以6 BV/h的流速洗脱并收集。验证试验结果表明，该工艺对雷公藤4种有效成分的总转移率在90％以上（RSD＝0.99％，n＝3）。结论：该优选纯化工艺稳定可行，适用于雷公藤4种有效成分的纯化。%OBJECTIVE:To study the purification technology of 4 active components from Tripterygium wilfordii by macropo-rous resin. METHODS:The purification abilities of nine macroporous resins(ADS-5,ADS-8,HPD100,HPD300,HPD400, HPD450,HPD700,HPD722 and HPD750) were studied with the adsorption and desorption rates of triptolide,wilforlide,trip-tonide and tripterine as the index by static adsorption and desorption experiments for 4 active components from T. wilfordii,so as to screen optimal macroporous resins. Using transfer rate of active component as index,single factor test was used to investigate the effects of different sampling method,ratio of mixing sample to total resin quantity,ratio of resin to medicinal material,cleaning so-lution(type,amount and cleaning flow rate),diameter- height ratio of resins,eluant(volume,flow rate)on adsorption,so as to determine the optimal elution technology;validation test was also conducted. RESULTS:HPD722 macroporous resin was chosen as adsorption resin;ratio of diameter to height was 1∶10,resin-medicinal material ratio was 1∶2,and ratio of mixing sample to to-tal resin quantity was 1∶10;wet column installing and mixing resin for sample loading were adopted. The macroporous resin was washed with 12 BV 20%ethanol at the rate of 12 BV/h,and then eluted with 12 BV 95%ethanol at the rate of 6 BV/h. The verifi-cation test results showed that the total transfer rate of 4 active components from T. wilfordii was more than 90%(RSD=0.99%, n=3). CONCLUSIONS:The optimized technology is stable and feasible,and suitable for the purification of 4 active components from T. wilfordii.