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Left ofloxacin and Pidotimod compound preparation tech and its appts.

A preparation process and technology of tea polyphenols, which are applied in the field of preparation process and device of high-purity tea polyphenols and monomeric catechins, can solve the problems of polluting resin columns, complicated process, single separation components, etc., and achieve Save time and equipment, high product yield, and high separation efficiency

Inactive Publication Date: 2005-01-12
胡绍海
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AI Technical Summary

Problems solved by technology

The solvent extraction method uses chloroform to extract the filtrate to remove pigment and caffeine; the precipitation method uses heavy metal ions to precipitate tea polyphenols in the filtrate to separate them from pigments and caffeine. These two methods may lead to organic Solvents or heavy metals remain, and the purity of the prepared tea polyphenols is not high
The methods for separating and extracting catechins from crude tea polyphenols include supercritical CO2 extraction, which has high product purity, but the process is complicated, the separation components are single, inconvenient to operate, and high in cost; liquid phase preparative chromatography and countercurrent chromatography, preparation The tea polyphenol monomer isolate has high purity and good recovery effect, but the investment cost is high, and the production capacity is "gram level", so it is difficult to expand the scale
Chinese patent 02113680.7 proposes a "production process for extracting pure catechins from tea". This patent uses D101 macroporous adsorption resin, but before the tea extract is put on the column, it only adjusts the pH value to precipitate fine particles and then filters them. Particles are difficult to remove, which will pollute the resin column and affect the adsorption effect; only a mixture of catechins with a purity of 90% can be produced after two column loadings, which increases the cost; and the toxic solvent chloroform is used
Chinese patent 00128567.x proposes "a separation method for catechin compounds in tea polyphenols", using glucose Sephadex LH-20 gel series columns, can obtain monomeric ester-soluble catechins EGCG, ECG, but single The purity of the body only reaches 90-95%, which cannot meet the requirements of pharmaceuticals. It is eluted with acetone and ethanol binary solvents, which is inconvenient for solvent recovery and increases production costs.
Chinese patent 01201087.1 proposes "a macroporous adsorption resin column", and 02256069.6 proposes a "macroporous resin ultrasonic natural drug adsorption separator". Their common problem is that the filter screen is clogged or the resin has been used for a long time and needs to be replaced with a new resin. It can only be dug out manually, which is time-consuming and labor-intensive, and basically these two kinds of equipment cannot be used for the separation and extraction of high-purity monomeric catechins.

Method used

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  • Left ofloxacin and Pidotimod compound preparation tech and its appts.

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1 Carry out according to aforementioned extraction process step, sedimentation centrifugation adopts DHC-500 type sedimentation disc separator (the following examples are the same), takes by weighing 150 kilograms of secondary dry green tea leaves, pulverizes to particle size≤1mm, presses tealeaves and pure The weight ratio of water is 1:8~15 (preferably 1:10), the temperature is 90~95°C, add pure water and stir for extraction for 10~20 minutes, and the weight ratio of filtered tea leaves: hot pure water is 1:4 ~6 (preferably 1:5), wash the slag once with hot pure water at 90~95°C, add hydrochloric acid or acetic acid to the tea extract twice to adjust the pH value to 3~4, after sedimentation and separation, the net liquid is adsorbed on the resin column, and the pure After washing the column with water, use ethanol with a weight concentration of 80% to desorb and elute tea polyphenols, control the adsorption flow rate to 8-16 liters / minute (preferably 8 liter...

Embodiment 2

[0033] Example 2 Take 150 kilograms of sub-dried green tea leaves and pulverize them to a particle size of ≤1 mm, add them to an extraction tank at a weight ratio of 1:5 to 8 (preferably 1:7) between tea leaves and 80% ethanol (or methanol), stir and extract for 25 to 10 mm. 35 minutes (preferably 30 minutes), control temperature 60 ~ 65 ℃, extract twice. Press filter to obtain the extract, adjust the pH value to 3-4 with hydrochloric acid (or acetic acid) and then settle and separate. After the liquid and water phases were separated by sedimentation and centrifugation, they were vacuum concentrated to recover ethyl acetate, and the solution phase was sprayed or freeze-dried to obtain a light yellow-white crude product of tea polyphenols. After HPLC analysis, the extraction rate was 13.21% of that of dry tea leaves, and the purity of crude tea polyphenols was ≥73.5%

[0034] Weigh 25 kg of alcohol-extracted crude tea polyphenols, add pure water to dissolve at 1:40 as in Examp...

Embodiment 3

[0035] Example 3 Weigh 25 kg of commercially available crude tea polyphenols, dissolve in pure water at a ratio of 1:50 as in Example 1, and then settle and separate to obtain a net liquid with carbon 18 (C 18 ) resin column adsorption, the control adsorption flow rate is 16 liters / minute, the desorption eluent methanol is added by a gradient of 1% per minute, and the elution gradient interval is 15% to 55%, only one elution is performed, and at the same time in pure water Add 0.05% TFA to the mixture, the desorption flow rate is constant at 9 liters / min, and the peak liquid of each monomer catechin is regularly collected according to the peak collection process in Example 1: EGC liquid is collected between 11 and 13 minutes, and DL is collected between 13.5 and 14.5 minutes -C solution, collect EGCG solution between 15 and 19 minutes, collect EC solution between 19.5 and 21 minutes, collect CAF solution between 21.5 and 25 minutes, collect GCG solution between 26 and 28 minute...

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Abstract

Tea leaves is used as raw material, by using water or solvent, to extract tea-polyphenol, then settle, centrifugal separation, column absorbing, extracting by ethyl acetate, vacuum concentrating, drying to obtain crude tea-polyphenol. Said crude product is then dissolved in water, absorbed by resin column, washed-off by agent gradient adding-in, based-on standard flowing curve to obtain 7 monomer catechins with purity>99%. For this purpose, full automatic absorbing resin column is equiped with metering pump to adjust fed-in of water, solution and solvent, HPLC real-time monitoring and pick-correcting to washing-off liquid is achieved by proportional flow-splitter. Automatic back-wash and resin-exchanging are achieved by being equiped with over-flow hole, resin discharging hole and others.

Description

technical field [0001] The invention relates to a process for extracting tea polyphenols and catechins from tea leaves and extraction equipment thereof, in particular to a process for preparing high-purity tea polyphenols and high-purity monomeric catechins by using an adsorption resin column and the adopted adsorption resin column. Background technique [0002] Tea polyphenols are a class of polyphenolic compounds extracted from tea leaves with catechins as the main body. They have the functions of anti-tumor, cancer prevention, lowering blood pressure and blood sugar, and inhibiting and killing pathogenic bacteria and viruses. Monomer epigallocatechin gallate (EGCG), which is isolated from tea polyphenols, is internationally recognized as "the first plant extracted after paclitaxel" due to its excellent anti-oxidation and anti-cancer properties. The most ideal new anti-cancer drug." Therefore, the process research and the development of extraction equipment for extracting ...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 胡绍海胡卫东万冰清
Owner 胡绍海
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