Camellia nitidissima saponin A, and preparation method and antitumor application thereof
A technology of tea saponin and golden camellia, which is applied in the field of camellia saponin A compound, can solve the problems of rough process, complex components, and inability to determine the composition and structure of components
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[0052] One, the preparation of camellia saponin A
[0053] 1. Instruments and reagents
[0054] Instrument: Intelligent Ultrasonic Extractor (Shanghai Zhixin Instrument Co., Ltd.).
[0055] Rotary evaporator (Shanghai Yarong Biochemical Instrument Factory)
[0056] Waters2695 High Performance Liquid Chromatography (Waters, USA)
[0057] Nicolet 4700 Fourier transform infrared spectrometer (KBr tablet, Nicolet company)
[0058] UV spectrophotometer (Thermo company)
[0059] AV600 nuclear magnetic resonance spectrometer (Bruker, Switzerland)
[0060] High-resolution time-of-flight mass spectrometer (Bruker, Switzerland)
[0061] Reagent: XAD-16 macroporous adsorption resin (Tianjin Haiguang Chemical Co., Ltd.)
[0062] D101 Macroporous Adsorption Resin (Nankai University Chemical Plant)
[0063] AB-8 macroporous adsorption resin (Nankai University Chemical Plant)
[0064] HP-20 macroporous adsorption resin (Mitsubishi, Japan)
[0065] Silica gel for chromatographic colu...
Embodiment 1
[0072] Put the golden camellia raw materials that have been prepared from the Shiwandashan Lanshan area of Fangchenggang City, Guangxi into the ultrasonic extractor, and put the methanol-water solution with a volume ratio of 50:50 according to the solid-liquid ratio of 1:10, and then put it under the condition of 40 ° C. Under the condition of leaching at 15KHz for 1h, the Camellia japonica extract was obtained.
[0073] Concentrate Camellia japonica extract, add water to dissolve, and absorb macroporous resin XAD-16 to obtain macroporous resin adsorbate.
[0074] The macroporous resin adsorbate was eluted with water for 5 column volumes, and then eluted with 70% ethanol, and the 70% ethanol part was collected and evaporated to dryness to obtain the total saponins of Camellia japonica; Separation by column chromatography, eluting with chloroform-methanol at a volume ratio of 15:1, and then taking the eluent for thin-layer chromatography detection, combining 123 to 162 fracti...
Embodiment 2
[0077] Put the prepared raw materials of Fangcheng Dawangjiang golden camellia tea into the ultrasonic extractor, put into the ethanol-water solution with a volume ratio of 55:45 according to the ratio of solid to liquid ratio of 1:12, and then soak at 50°C at 20KHz Extract for 2 hours to obtain Camellia Camellia extract.
[0078] Concentrate Camellia japonica extract, add water to dissolve, and absorb macroporous resin D101 to obtain macroporous resin adsorbate.
[0079] The macroporous resin adsorbate was eluted with water for 5 column volumes, and then eluted with 70% ethanol, and the 70% ethanol part was collected and evaporated to dryness to obtain the total saponins of Camellia japonica; Separation by column chromatography, eluting with chloroform-methanol with a volume ratio of 17:2, and then taking the eluent for thin-layer chromatography detection, combining 123-162 fractions and concentrating to obtain a concentrated solution, and concentrating the concentrated solut...
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