CN112494473A - Soy sauce head extract and preparation method and application thereof - Google Patents
Soy sauce head extract and preparation method and application thereof Download PDFInfo
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- A61K31/19—Carboxylic acids, e.g. valproic acid
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Abstract
The invention provides a method for extracting a Soy sauce head extract, which comprises the following steps: (1) crushing: pulverizing the Chinese medicinal sauce head with a pulverizer, and sieving; (2) weighing certain parts of sauce head powder, adding a solvent, soaking and extracting for 2 days at room temperature, filtering and collecting an extracting solution, soaking and extracting filter residues for 2-3 times, combining the extracting solutions, spin-drying by a rotary evaporator, drying at 50 ℃ to constant weight, adding water, ultrasonically dissolving and uniformly mixing, adding ethyl acetate, extracting for 2-3 times, combining the extracting solutions, and concentrating under reduced pressure to obtain an extract; (3) and (3) carrying out elution separation on the extract by adopting normal phase silica gel column chromatography, taking dichloromethane and methanol with a certain proportion as an elution solution, collecting the eluent, concentrating under reduced pressure, and drying at 50 ℃ to constant weight. The Maotai extract obtained by the method provided by the invention contains 5 phenolic acid substances with higher content, and the extract has better protection effect on gastric epithelial cells.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, and particularly relates to a sauce head extract and a preparation method and application thereof.
Background
The sauce head is common Chinese herbal medicine for Yi nationality in Yunnan province, and is derived from root tuber of Fallopia dentata of Polygonum of Polygonaceae. It is astringent and cool in nature and taste, has astringent, antidiarrheal, antiinflammatory, and analgesic effects, and can be decocted or pulverized into powder for oral administration for treating dysentery, dyspepsia, and chronic hepatitis; it can be administered with wine for internal hemorrhage; the fresh product is mashed or the dry powder is externally applied to the early stage of furuncle, traumatic bleeding and the like, and the Yi nationality uses the root tuber thereof to treat chronic hepatitis with good curative effect.
Gastric bleeding is a relatively serious condition, which often occurs when some stomach diseases are suffered, and causes of gastric bleeding are gastric cancer, heavy drinking, gastric ulcer, acute damage to gastric fascia and the like, wherein gastric ulcer and damage to gastric fascia are the most common. Gastric ulcer is an ulcer caused by an imbalance between defense factors and attacking factors of the gastric mucosa, and occurs between the pylorus and cardia of the stomach. The gastric ulcer is a digestive system disease with high morbidity, and the detection rate of the gastric ulcer in each part of China per year reaches 16-33%. Common complications of gastric ulcer include upper gastrointestinal bleeding, ulcer perforation, pyloric obstruction, canceration, etc. In addition, the application of non-steroidal anti-inflammatory drugs, alcoholism, helicobacter pylori invasion and the like can cause gastric ulcer, and the gastric mucosa is damaged.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a sauce head extract and a preparation method and application thereof.
A method for extracting Soy sauce head extract comprises the following steps:
(1) crushing: pulverizing the Chinese medicinal sauce head with a pulverizer, and sieving;
(2) weighing certain parts of sauce head powder, adding a solvent, soaking and extracting for 2 days at room temperature, filtering and collecting an extracting solution, soaking and extracting filter residues for 2-3 times, combining the extracting solutions, spin-drying by a rotary evaporator, drying at 50 ℃ to constant weight, adding water, ultrasonically dissolving and uniformly mixing, adding ethyl acetate, extracting for 2-3 times, combining the extracting solutions, concentrating under reduced pressure to obtain an extract, carrying out elution separation on the extract by adopting normal phase silica gel column chromatography, taking dichloromethane and methanol in a certain proportion as an elution solution, combining the eluates according to a TLC detection result, concentrating by the rotary evaporator, and drying at 50 ℃ to constant weight.
Further, according to the extraction method of the Maotai extract, the screening mesh number in the step (1) is 40-60 meshes.
Further, according to the extraction method of the Maotai extract, in the step (2), the solvents are ethanol/water solutions with different proportions, and the volume fractions of the ethanol and the water solutions are 0-95%.
Further, according to the extraction method of the Maotai extract, the mass ratio of the Maotai powder to the solvent in the step (2) is 1: 5-1: 20.
Further, according to the extraction method of the Maotai extract, the mass ratio of the Maotai extract to water in the ultrasonic dissolving in the step (2) is 1: 20-1: 50, and the mass ratio of the water to the ethyl acetate is 2: 1-1: 3.
Further, according to the extraction method of the Soy sauce head extract, the volume ratio of the dichloromethane to the methanol in the step (2) is 9: 1-7: 3.
The resulting soy sauce head extract is extracted according to any of the methods described above.
According to the extract, the extract contains gallic acid, ethyl 3, 4-dihydroxybenzoate, Su-1-C-eugenol glycerol, catechin (+) and cannabinamide F, namely the compounds shown in formula I, formula II, formula III, formula IV and formula V, which are detected by HPLC:
the use of the Maotai extract as described above in the preparation of a gastric epithelial cell protectant.
Has the advantages that:
1. the method provided by the invention can fully extract the effective components of the sauce head. The extraction method provided by the invention is simple to operate, has high extraction efficiency, and can fully extract the effective components of the traditional Chinese medicine, so that the effective utilization value of the traditional Chinese medicine sauce is improved. The extract obtained by the extraction method can be used for preparing gastric mucosa protective agent.
2. The prepared sauce head extract contains gallic acid, catechin (+), cannabinamide F, Sushi-1-C-eugenol glycerol and 3, 4-dihydroxy ethyl benzoate, and the phenolic acid components are natural antibacterial anti-cancer anti-inflammatory drugs, have small toxic and side effects, and can be used for preparing a gastric epithelial cell protective agent.
Drawings
FIG. 1 is a comparative HPLC chart of the mixed control and sample of example 2;
wherein A: HPLC chromatogram of the mixed control, B: HPLC chromatogram of the extract of soy sauce;
1-gallic acid, 2-catechin (+), 3-cannabinamide F, 4-threo-1-C-eugenol glycerol, and ethyl 5-3, 4-dihydroxybenzoate;
FIG. 2 is a graph showing the content of 5 phenolic acid components in different Soy extract of example 2;
FIG. 3 is a graph showing the effect of different concentrations of ethanol extracts on the viability of GES-1 cells;
drawing notes: a is 0% ethanol extract of Soy sauce head; b is a sauce head extract extracted by 50% ethanol; a is a sauce head extract extracted with 95% ethanol; the low dose was 0.2. mu.g/mL and the high dose was 1.0. mu.g/mL.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides an extraction method of a Maotai extract, which comprises the following steps:
(1) crushing: pulverizing the Chinese medicinal sauce head with a pulverizer, and sieving;
(2) weighing 300g of crushed sauce head, adding 1.5L of ethanol (0%, 50% and 95%) with different concentrations, soaking and extracting for 2 days at room temperature, filtering and collecting extract, soaking and extracting filter residues for 2-3 times, combining the extract, concentrating by a rotary evaporator, drying at 50 ℃ to constant weight, adding water, ultrasonically dissolving and uniformly mixing, adding ethyl acetate, extracting for 2-3 times, combining the extract, concentrating under reduced pressure to obtain an extract, eluting and separating the extract by using normal phase silica gel, sequentially eluting by using dichloromethane/methanol (volume ratio of 9:1, 8:2 and 7:3), collecting eluent, concentrating under reduced pressure, and drying at 50 ℃ to constant weight to obtain the sauce head extract.
Table 1 influence of different concentrations of ethanol on the yield of the Maotai extract (n ═ 3)
| Concentration of ethanol | Soy sauce head extract yield (%) |
| 0% ethanol | 3.7±0.3 |
| 50% ethanol | 5.3±0.6 |
| 95% ethanol | 6.5±0.9 |
Example 2
Measuring the content of gallic acid, catechin (+), cannabinamide F, Sushi-1-C-eugenol glycerol and ethyl 3, 4-dihydroxybenzoate in the sauce head extract by high performance liquid chromatography.
The contents of gallic acid, catechin (+), cannabinamide F, Su-1-C-eugenol glycerol and ethyl 3, 4-dihydroxybenzoate in the 3 kinds of sauce head extracts prepared in example 1 by different extraction methods were measured by high performance liquid chromatography, and the specific contents were as follows:
the instrument comprises the following steps: shimadzu high performance liquid chromatograph (comprising on-line degasser DGU-20A3R (C), binary pump LC-20AB, autosampler SIL-20A, column oven CTO-20A, detector SPD-20A).
(1) Chromatographic conditions are as follows:
a chromatographic column: welchrom C18Chromatography column (5 μm, 4.6X 250 mm); mobile phase: the solution A is 0.5 percent phosphoric acid solution, and the mobile phase solution B is methanol; flow rate: 1.0mL min-1; column temperature: 30 ℃; detection wavelength: 210 nm; sample introduction amount: 10.0 μ L; gradient elution conditions: 0-15 min, 10-30% of B; 15-35 min, 30-40% B; 35-50 min, 40-70% B;
(2) preparation of Mixed control solution
2.6, 4.6, 1.6 and 2.9mg of gallic acid, catechin (+), cannabinamide F, Sushi-1-C-eugenol glycerol and 3, 4-dihydroxy ethyl benzoate are precisely weighed respectively and placed in a 1mL volumetric flask respectively, and methanol is added to scale marks to prepare mixed reference solutions with mass concentrations of 2.6, 4.6, 1.6 and 2.9mg/mL respectively.
(3) Preparation of test solution
2mg of the 3 kinds of Soy head extracts in example 1 were precisely weighed, dissolved by adding methanol, and made to a volume of 10mL, and filtered through a 0.45 μm filter membrane to obtain a test solution.
(4) Drawing of standard curve
Preparing 5 different concentrations of the mixed reference substance, respectively and precisely sucking 10 μ L of the mixed reference substance solution, injecting into a high performance liquid chromatograph, performing HPLC determination according to the chromatographic conditions in the step (1), and drawing a standard curve by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate.
(5) Content determination of 5 phenolic acid substances in test sample
And (3) detecting the test solution by adopting the chromatographic conditions in the step (1), and calculating the content of 5 phenolic acid substances in the test according to the standard curve drawn in the step (4).
FIG. 1 is a comparative HPLC chart showing the mixed control and sample of example 2, and it can be seen from FIG. 1 that the Soy extract prepared in this example has the effect of protecting gastric epithelial cells, and is related to the 5 phenolic acid components contained therein.
FIG. 2 is a graph showing the content of 5 phenolic acid components in different Soy extract of example 2 (n-3); as can be seen from fig. 2, the three types of extract from the sauce head extracted with ethanol of different concentrations all contain 5 types of phenolic acid components, i.e., gallic acid, catechin (+), cannabinamide F, threo-1-C-eugenol glycerol, and ethyl 3, 4-dihydroxybenzoate, wherein the contents of gallic acid, cannabinamide F, and threo-1-C-eugenol glycerol are relatively high, and the sum of the contents of the 5 types of phenolic acid components in the extract from the sauce head extracted with 50% ethanol is the highest among the three types of extract from the sauce head.
Example 3
The protective effect of Maotai effective components on gastric epithelial cells, the present example studies the protective effect of Maotai extract on the damage of GES-1 gastric epithelial cells caused by ethanol.
(1) Subculturing of cells
DMEM culture solution containing 10% fetal calf serum and 5% CO at 37 DEG C2GES-1 (human gastric epithelial cells) was cultured under the conditions. When the cells grew to the bottom of the flask, trypsin was added to the flask for digestion and passaging.
(2) Cell grouping and modeling
The cells were divided into 9 groups, i.e., normal group, model group, positive control group (ranitidine 0.1. mu.g/mL), low dose (3 kinds of extract of Soy sauce at a concentration of 0.2. mu.g/mL), high dose (3 kinds of extract of Soy sauce at a concentration of 1.0. mu.g/mL). The serum concentration in the culture medium was 10% for each group. Except the normal group, 1% ethanol was added to each of the other groups for molding.
(3) Cell viability assay
The survival rate of gastric epithelial cells was calculated by measuring the absorbance at 490nm using an enzyme-labeling instrument using the MTT method.
As can be seen from FIG. 3, after the molding with 1% ethanol, the activity of gastric epithelial cells is reduced, and the Maotai extract extracted with 50% ethanol and 95% ethanol has a certain repairing effect on ethanol-induced cell damage, and the cell activity is obviously enhanced with the increase of dosage.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The extraction method of the sauce head extract is characterized by comprising the following steps:
(1) crushing: pulverizing the Chinese medicinal sauce head with a pulverizer, and sieving;
(2) weighing certain parts of sauce head powder, adding a solvent, soaking and extracting for 2 days at room temperature, filtering and collecting an extracting solution, soaking and extracting filter residues for 2-3 times, combining the extracting solutions, spin-drying by a rotary evaporator, drying at 50 ℃ to constant weight, adding water, ultrasonically dissolving and uniformly mixing, adding ethyl acetate, extracting for 2-3 times, combining the extracting solutions, concentrating under reduced pressure to obtain an extract, carrying out elution separation on the extract by adopting normal phase silica gel column chromatography, taking dichloromethane and methanol in a certain proportion as an elution solution, combining the eluates according to a TLC detection result, concentrating by the rotary evaporator, and drying at 50 ℃ to constant weight.
2. The extraction method of the Maotai extract as claimed in claim 1, wherein the mesh number of the screen in the step (1) is 40-60 meshes.
3. The extraction method of the Maotai extract as claimed in claim 1, wherein the solvent in the step (2) is ethanol/water solution with different ratio, and the volume fraction of the ethanol/water solution is 0-95%.
4. The extraction method of the Soy sauce head extract as claimed in claim 1, wherein the mass ratio of the Soy sauce head powder to the solvent in the step (2) is 1: 5-1: 20.
5. The extraction method of the Maotai extract as claimed in claim 1, wherein the mass ratio of the Maotai extract to water in the ultrasonic dissolution in the step (2) is 1: 20-1: 50, and the mass ratio of the water to the ethyl acetate is 2: 1-1: 3.
6. The extraction method of the Maotai extract as claimed in claim 1, wherein the volume ratio of dichloromethane to methanol in the step (2) is 9: 1-7: 3.
7. A Maotai extract obtained by extraction according to the method of any one of claims 1 to 6.
8. The extract of claim 7, wherein the extract contains gallic acid, ethyl 3, 4-dihydroxybenzoate, threo-1-C-eugenol glycerol, catechin (+) and cannabinamide F as measured by HPLC, i.e., compounds of formula I, formula II, formula III, formula IV and formula V:
9. use of the Maotai extract according to claim 7 for the preparation of a gastric epithelial cell protectant.
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| JP2003073264A (en) * | 2001-09-04 | 2003-03-12 | Taiho Yakuhin Kogyo Kk | Antiulcer agent |
| CN104622994A (en) * | 2015-03-13 | 2015-05-20 | 王磊 | Pharmaceutical composition for treating chronic gastritis |
| US20170119772A1 (en) * | 2015-10-30 | 2017-05-04 | Botamedi Inc. | Beverage composition comprising phlorotannin, ginseng extract and caffeine |
| CN109200103A (en) * | 2017-07-07 | 2019-01-15 | 海南皇隆制药股份有限公司 | The preparation method of daphniphyllum calycinum and Herba polygoni hydropiperis extract |
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|---|---|---|---|---|
| JP2003073264A (en) * | 2001-09-04 | 2003-03-12 | Taiho Yakuhin Kogyo Kk | Antiulcer agent |
| CN104622994A (en) * | 2015-03-13 | 2015-05-20 | 王磊 | Pharmaceutical composition for treating chronic gastritis |
| US20170119772A1 (en) * | 2015-10-30 | 2017-05-04 | Botamedi Inc. | Beverage composition comprising phlorotannin, ginseng extract and caffeine |
| CN109200103A (en) * | 2017-07-07 | 2019-01-15 | 海南皇隆制药股份有限公司 | The preparation method of daphniphyllum calycinum and Herba polygoni hydropiperis extract |
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