A method for preparing high-purity hydroxytyrosol by high-speed countercurrent chromatography and high-performance liquid chromatography
A technology of high-speed countercurrent chromatography and high-performance liquid chromatography, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of high-purity hydroxytyrosol in batches, and achieve fewer steps, high cost, and high production efficiency. rate-enhancing effect
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Embodiment 1
[0032] Embodiment 1 high-speed countercurrent chromatography standard sample separation
[0033] 1. Experimental equipment:
[0034] FastChrome analytical high-speed countercurrent chromatography (Jiangyin Countercurrent Technology Co., Ltd.); separation column volume: 25ml; value range: 0.56 to 0.91; OptiChromeA semi-preparative high-speed countercurrent chromatography (Jiangyin Countercurrent Technology Co., Ltd.); spiral tube separation column (revolution Radius: 80cm; value range: 0.50~0.80; spiral tube inner diameter: 1.59mm), single column volume 180ml, double column volume 360ml.
[0035] 2. Experimental materials:
[0036] Analysis of pure isomer phenolic samples catechol, resorcinol, hydroquinone; n-hexane, ethyl acetate, methanol, distilled water
[0037] 3. Preparation of solvents and samples:
[0038] Prepare methanol mixed solution of phenolic samples, mixed sample concentration: catechol 20mg / ml + resorcinol 20mg / ml + hydroquinone 10mg / ml; use 80% methanol sol...
Embodiment 2
[0059] Embodiment 2 high-speed countercurrent chromatography and high-performance liquid chromatography combined method
[0060] The first step, preparation of hydroxytyrosol ointment
[0061] The olive leaf oleuropein extract is enzymatically hydrolyzed, the solid-liquid ratio of the extract to 4-7 phosphate buffer solution is 1g: 10-100mL, the mass ratio of the extract to biological enzyme is 1g: 20-100mg, placed in 30 ℃ ~ 100 ℃ constant temperature water bath shaker. After enzymatic hydrolysis for 1h-10h, filter, the filtrate is extracted with ethyl acetate, the ethyl acetate layer is concentrated and dried, the concentrate is hydroxytyrosol ointment, the yield of ointment relative to plant leaf powder is 1-20%, and the content of hydroxytyrosol is 5-20%. 20%;
[0062] The second step, high-speed countercurrent chromatographic separation
[0063] 1) Select petroleum ether: ethyl acetate: methanol: water as 3~6:4~8:3~6:4~8 solution according to the volume ratio as the hig...
Embodiment 3
[0068] Example 3 High Speed Countercurrent Chromatography Separation of Hydroxytyrosol Ointment Experiment
[0069] 1. Solvent preparation: petroleum ether: ethyl acetate: methanol: water = 2:3:2:3, prepare 2000ml according to the volume ratio, the upper phase is the stationary phase, and the lower phase is the mobile phase.
[0070] 2. Sample preparation: Take 50 mg of hydroxytyrosol ointment in Example 3 and dissolve it in 50 ml of mobile phase.
[0071] 3. System balance: pump the stationary phase at a speed of 50ml / min, pump the mobile phase at a speed of 5ml / min, and start
[0072] 4. OptiChrome TM A-300 is centrifuged forward, observe that the output of UV3000 reaches the system balance, and calculate the stationary phase retention rate: 60%
[0073] 5. Sample loading: inject the sample into OptiChrome through the sample loading valve TM A-300 in. Forward centrifugation: OptiChrome TM A-300 is set to positive centrifugal rotation, setting. The sample is obtained ...
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