Extract Polyglycosides From Tripterginum Wilfordii Hook. F And Its Micronization

Tripterygium Wilfordii Hook.f.(T. Wilfordii)is a kind of traditional Chinese medicine,which has immunosuppressive effect.Methods are established to determine the content of polyglycosides and triptolide. Operating procedures of traditional methods are trival and the content of the main actives component in the extracts are very low. This paper take the method of pressurized liquid extraction to extract polyglycosides from Tripterygium wilfordii Hook.f for the first time. And make a comparative analysis with traditional methods for extracting, then polyglycosides were entrapped into micro powder by the application of supercritical solvent.And analyse the performance characterization.These researches can improve the efficacy of the medicine and promote themodernization traditional Chinese medicine industry. The main research contents are as follows:1. A reliable and stable method is established to determine the content of polyglycosides and triptolide.Polyglycosides is determined by the method of colorimetry.The appropriate detection conditions were:519nm detected wavelength, colour-display reagent: 1%3,5-2 nitrate benzoic acid dissolved in ethanol and 1 %NaOH solution.the determination of triptolide by the method of HPLC, conditions:Chromatographic column:Hypersil BDS C18(5μm,4.6 mm×250 mm),mobile phase:ethanol-water(40:60,v/v),flow rate:1 mL/min, the temperature of column was 25℃, sample size:10μL, detected wavelength:218 nm. Through the investigation, the above two methods are up to the analysis of requirement.2. Take the method of pressurized liquid extraction to extract polyglycosides from Tripterygium wilfordii Hook.f. Taking the purity and the extract ratio as quality indexes, study the ratio of solid to liquid, extraction time, temperature on the impact of extraction, the optimized conditions were as followed:ratio of solid to liquid was 1:9.5 (g:mL),at the temperature of 115℃for 80 minutes, the purity and actual of extract ratio of polyglycosides obtained were 0.52% and 0.21% respectively. This research take the method of pressurized liquid extraction to extract polyglycosides from Tripterygium wilfordii Hook.f for the first time, And the results were very good.3. We also make a comparative analysis with traditional methods, The results showed the method of pressurized liquid extraction is only a little lower than Ethanol refluxing-Neuter alumina adsorption-chloroform extraction in the purity,and the extract ratio up to 86.4%.The purity of the method of Ethanol refluxing-chloroform extraction is only 0.23%.The method of water-Ethanol extraction both lower in the purity and the extract ratio.The extract ratio of triptolide of pressurized liquid extraction up to 0.173%o, the highest of the four experiments. Thus, we can see the method of pressurized liquid extraction have obviously advantages over traditional extract methods in the purity and extract ratio.4. Supercritical antisolvent (SAS) process is taken to prepare the micro particles of polyglycosides, with ethanol as solvent, taking the size of micro particles as quality indexes. Study precipitation pressure,concentration of solution,drag solution on flow rate,precipitation temperature, flow rate of CO2.The best technological conditions obtained were as followed: precipitation pressure:25Mpa, concentration of solution:21.6 mg/ml, drag solution on flow rate: 6ml/min, precipitation temperature:55℃, flow rate of CO2:20kg/h. the minimum size of micro particles reach 810nm. But, the demand for equipment is higher, and the equipment operation procedure is complicated, the feasibility of industrial still needs to be further discussed.5. For the further study of micro particles,the performance characterization were analysed.Results:the scanning electron microscopy images on the micro particles were observed in 820nm, spherical.The molecular structures of raw Tripterygium and polyglycosides micro particles were examined with FTIR, no significant differences were observed between the two samples. X-ray diffraction analyses show the raw tripterygium at the crystal level are lower than polyglycosides micro particles. From the analysis of TG-DTG respectively.We can see the temperature condition of supercritical is in the appropriate range. Solubility test results show that the solubility of micro powder is 2.1 times of raw materials. Thus,we can draw the conclusion that the bioavailability of micro powder may be increased, if micro powder used in drug as raw material, it can reduce patient medicine, thereby lowering the toxicity, but its pharmacological process still need further study.