烏索酸的生產(chǎn)工藝

第57卷第2期化工學(xué)報Vol. 57 No. 2006年2月Journal of Chemical Industry and Engineering China)ruar2006研究快報Production process for ursolic acidLI Kaiquan(李開(kāi)泉), CHEN WU(陳武), LI Xiangyi(李翔(Yichun College, Yichun 336000, Jiangxi, China)Abstract: Production of ursolic acid, the anti-hepatitis effective composition from natural plantSambucus chinensis Lindl. was carried out and the scale-up preparation technology was studiedExtraction of the herb sambucus chinensis lindl. was extracted in reflux with 7 volume times of refluxinethanol at 80C for 1 h for two times. The extract was purified with a selt-made specific impurity removerYCXY-1"to yield ursolic acid of high purity. A new"Extraction/Gelation"technology for the productionof ursolic acid was developed. The specific impurity remover"YCXY-1 "showed high effectiveness inpurification. The purity of the mass-produced ursolic acid was up to 99. 8%. The chemical structure of theproduct was confirmed by the physicochemical constants and spectroscopic identification. The productionof high-purity ursolic acid was optimized with natural plant as raw material and with only ethanol asextracting solvent. The difficulties such as isolation and impurity removal were addressed effectively. Thenovel technology is reasonable, convenient, practical, low-cost, high-yield, suitable for mass productionKey words: Sambucus chinensis lindl; ursolic acid; extraction and separation; production processCLC number: R 284. 2Document code: AArticle id:0438-1157(2006)02-0380-021.2 InstrumentstroductionHPLC. Beckman-126/168: FTIR. NicoletThe herb sambucus chinensis LindL. is an IMPACt-400:H NMR and C NMR, InOvAeffective medicine for treating hepatitis. According 500; Mass Spectrometer. Autospec-Ultima ETOFto studies in pharmacology experiment and clinic EI and Magnet BPI.practice, ursolic acid in Sambucus chinensis LindL. 1.3 Experimental stepsis the major effective component for anti-hepatitisDried herb raw powder of Sambucus chinensisactivity 1-3LindL. was extracted by 95 ethanol at 80C for 1h for 2 times. The two extracts were combined and1 Experimentsethanol was recycled under vacuum. The resulted1.1 Materialsslush was treated by impurity remover"YCXY-1Sambucus chinensis Lindl. is grown inseparated by gelation and then decolorized withYichun, Jiangxi Province, China. The standard active carbon. After purification and final air-sample of ursolic acid is provided by Chinadrying. colorless needle-like crystalline ursolic acidInstitute of Identification of Drug and biologicalProducts中國煤化工CNMHGReceived date: 2005-07-06First and corresponding author: PLI Kaiquan, maleThe sample was colorless needle-like crystalborn in 1954insoluble in water. La 2+65(c 0.095, EtOH)Foundation item: supported by the National High Technologyof meltingDevelopmen China(204A222observed when it was mixed with standard sample.第2期LI Kaiquan, et al: Production process for ursolic acid3812.2 Thin layer chromatographyThe sample was dissolved in methanol (2 mg2 mg ursolic acid was dissolved in 1 ml 95% ml ) 20 ul of the sample solution was injectedethanol, and the sample was applied to hard tlc into the apparatus. The chromatograms wereplate of silica sel G, along with standard sample as normalized by external standard method and gavecontrast. Mixture of cyclohexane and acetone (3the ursolic acid content of 99.82After air drReferencesplates were sprayed with 10% sulfuric acid inethanol and heated to 110C for10 min to develop[1 Li Kaiquan(李開(kāi)泉), Chen wu(陳武), Xiong Xiaojuanthe plate. It was found that both the purified(熊筱娟). Chemical research of ursolic acid -the anticomponent in Sambucus chinensis Lindl. Chinesesample and the standard sample showed the sameTraditional and Herbal Drugs(中草藥),2001,32purple-red spot under visible light or golden spotsuppl.):36-37der uv of 365nm and the same Re] Chen Wu(陳武), Li Kaiquan(李開(kāi)泉), Xiong Xiaojuan3 Identification of chemical structure熊筱娟). Research of the anti-hepatitis active component ofThe FtiR, EI-MS,H NMR,3C NMRinensis Lindl,. Journal of NanchangUniversity(南昌大學(xué)學(xué)報spectral data of sample agree with those of ursolic[a3] Song jing(宋京), Zhang Qinglin(張慶林). Developmentsacid reported in literatures 4-5JTraditional and Herbal Drugs(中草藥),1999,303 Content of ursolic acid( suppl.):196-198[4] Cong puzhu(叢浦珠). Application of Mass Spectroscopy inConditions for HPlC: Column. C18-ODS 150Organic Chemistry of Natural Products(質(zhì)譜學(xué)在天然有機4. 6 mm, 5 um: temperature,化學(xué)中的應用). Beijing: Science press,1987:684-686temperature; working wavelength, 2=210 nm[5] Peng Shiqi(彭師奇). Interpretation of Drug Spectroscopy(藥物的波譜解析). Beijing: Joint Press of Beijing Medicasensitivity, 0. 005 AUFS; mobile phase, methanolUniversity and Union Medical College, 1998water(88: 12); eluting speed. 1.0 ml.min中國煤化工CNMHG