CN115252661A - Purslane lactam extract and preparation method and application thereof - Google Patents
Purslane lactam extract and preparation method and application thereof Download PDFInfo
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- CN115252661A CN115252661A CN202210666106.XA CN202210666106A CN115252661A CN 115252661 A CN115252661 A CN 115252661A CN 202210666106 A CN202210666106 A CN 202210666106A CN 115252661 A CN115252661 A CN 115252661A
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Abstract
The invention discloses a purslane lactam extract and a preparation method and application thereof, wherein the total content of compounds I and II in the purslane lactam extract obtained by the invention is 75-84%, and the recovery rate is 0.15-0.21%, which is to separate and extract the two lactam components from purslane for the first time; the purslane lactam extract prepared by the invention has the activity of treating and relieving pulmonary hypertension, and has the advantages of simple process, convenient operation, less equipment investment, capability of being used for common food and the like;
Description
Technical Field
The invention relates to a purslane lactam extract, a preparation method thereof and application thereof in preparing a medicament for preventing and treating pulmonary hypertension.
Background
Herba Portulacae (Portulaca oleracea L.) is an annual herb of Portulaca of Portulacaceae, also called herba WUXINGCAO, herba Portulacae, and herba Benincasae; widely distributed in temperate and tropical regions. The purslane herb is edible and medicinal, has cold nature and sour taste, has the effects of clearing heat and promoting diuresis, detoxifying and reducing swelling, and cooling blood and stopping bleeding, and is listed as one of the most widely used medicinal and edible plants by the world health organization. Purslane has wide pharmacological activity, is used as a folk medicine in multiple countries, and is commonly used for treating diabetes, gastrointestinal diseases, promoting wound healing and other diseases
Pulmonary hypertension is a disease seriously endangering human life and health, and is mainly characterized by progressive increase of pulmonary vascular resistance, and most patients die of right heart failure within a year after diagnosis if the patients are not actively treated, so that the pulmonary hypertension is called as malignant tumor of a cardiovascular system. In recent years, western medicine has mainly used phosphodiesterase 5 (PDE 5) inhibitors, nitric oxide, endothelin receptor antagonists, prostacyclin drugs, and the like for the treatment of pulmonary hypertension. However, these drugs have either strong side effects or are expensive to treat, which imposes a heavy economic burden on patients. Researches on the theory and practice basis of the active ingredients of the traditional Chinese medicine for preventing and treating pulmonary hypertension provide good social and economic benefits. Early-stage research shows that the two lactam components in the purslane have better effects of preventing and treating pulmonary hypertension, and can improve the hemodynamic indexes of a rat model established by monocrotaline induction and have the effect of relaxing pulmonary vessels.
Disclosure of Invention
The invention aims to provide a purslane lactam component with the activity of preventing and treating pulmonary hypertension and a preparation method thereof.
The technical scheme of the invention is as follows:
a purslane lactam extract is prepared by the following method:
(1) Cleaning fresh purslane, drying, crushing and sieving (20 meshes) to obtain purslane powder, and extracting with ethanol to obtain extract;
specifically, the ethanol leaching method comprises the following steps: mixing purslane powder with ethanol in a mass ratio of 1:7-9, stirring and soaking at room temperature for 1-3 h, heating to 70-100 ℃, performing reflux extraction for 0.5-3 h, cooling to 30-50 ℃, filtering to obtain filtrate, namely purslane alcohol extract, and concentrating under reduced pressure until no ethanol smell exists to obtain an extract;
(2) Dispersing the extract obtained in the step (1) with water, adding chitosan, stirring at room temperature for 2-6 h, then centrifuging, and removing precipitates to obtain a supernatant; adding an extracting agent into the supernatant to obtain a mixed solution, stirring the mixed solution for 30 to 90min at the temperature of between 50 and 80 ℃ for extraction, then cooling the mixed solution to between 30 and 40 ℃, standing and layering the mixed solution to obtain an upper layer of extract liquor and a lower layer of raffinate, and concentrating the upper layer of extract liquor under reduced pressure to obtain a purslane crude extract;
preferably, the extract is dispersed by water with the volume of 20-30 times;
preferably, the addition amount of the chitosan is 1/200-1/300 of the mass of the purslane powder, and the chitosan is used for removing polyphenol and other impurities in the extract;
the centrifugation conditions were: centrifuging at 5000-10000 rpm at 20 ℃ for 5-10 min;
the extractant is formed by mixing an organic solvent A and an organic solvent B according to the volume ratio of 500.5-5, wherein the organic solvent A is a mixed solution of ethyl acetate and n-butanol according to the volume ratio of 1-3:1; the organic solvent B is acetic acid; the organic solvent A and the organic solvent B have no special meaning, and are marked as A and B only used for distinguishing different organic solvents; preferably, the volume of the extracting agent is 10 to 20 times of that of the extract;
preferably, the upper layer extract is decompressed and concentrated to 0.02 to 0.05 time of the volume of the mixed solution;
(3) Adding the purslane crude extract obtained in the step (2) into a chromatographic column filled with polyvinylpyrrolidone at the speed of 0.02-0.08 BV/min, eluting with 2-5 BV of distilled water until the effluent is colorless, eluting with 70-80% ethanol aqueous solution with the volume concentration of 3-5 BV, collecting the eluate, and concentrating under reduced pressure to remove the solvent to obtain a purslane lactam extract;
the preferred column chromatography operation is: adding the purslane crude extract obtained in the step (2) into a chromatographic column filled with polyvinylpyrrolidone at the speed of 0.03-0.05 BV/min, eluting with 2-4 BV of distilled water until the effluent is colorless, eluting with 70-80% ethanol aqueous solution with the volume concentration of 3-4 BV, collecting the eluent, and removing the solvent by concentration under reduced pressure to obtain the purslane lactam extract.
The purslane lactam extract prepared by the invention mainly contains compounds shown in the following formulas I and II:
COMPOUND I R＝H
COMPOUND II R＝OCH3
the total amount of the two compounds I and II accounts for more than 75% of the total mass of the purslane lactam extract.
The purslane lactam extract prepared by the invention can be used for preparing medicines for preventing and treating pulmonary hypertension.
Compared with the prior art, the invention has the following beneficial effects:
(1) In the purslane lactam extract obtained by the method, the total content of the compounds I and II is 75-84%, and the recovery rate is 0.15-0.21%; the two lactam components are obtained by separating and extracting the purslane for the first time.
(2) The purslane lactam extract prepared by the invention has the activity of treating and relieving pulmonary hypertension.
(3) The method has the advantages of simple process, convenient operation, less equipment investment, and the product can be used for common food.
Drawings
FIG. 1 liquid chromatogram of Portulaca oleracea lactam extract prepared in example 1.
Figure 2 Right Ventricular Systolic Pressure (RVSP) of rats in each group of example 2.
FIG. 3 mean pulmonary arterial pressure (mPAP) in each group of rats in example 2.
Detailed Description
The invention is further described below by means of specific examples, without the scope of protection of the invention being limited thereto.
Example 1
Weighing 500g of purslane powder crushed into 20 meshes, putting the purslane powder into a round-bottom flask, adding 4L 75% ethanol, stirring and soaking for 3 hours at room temperature (25 ℃), then heating and refluxing for leaching for 3 hours at 100 ℃, cooling reaction liquid to 30 ℃, filtering, taking filtrate to obtain purslane alcohol extract, and concentrating the purslane alcohol extract to 100mL in rotary evaporation (0.09MPa, 60 ℃) under reduced pressure; dispersing the concentrate with 2L water, adding 2g chitosan, stirring at room temperature for 3 hr, centrifuging at 20 deg.C at 5000 rpm for 5 min to remove precipitate, and collecting supernatant; transferring the supernatant into a round-bottom bottle, adding 0.8L ethyl acetate, 0.7L n-butanol and 2mL acetic acid into the round-bottom bottle to prepare a mixed solution, stirring and extracting the mixed solution at 70 ℃ for 60 minutes, cooling to 40 ℃, placing the cooled mixed solution into a separating funnel, standing for 30 minutes, and layering to obtain an upper layer extract and a lower layer raffinate; concentrating the upper layer extractive solution on rotary evaporator (0.09MPa, 55 deg.C) under reduced pressure to 100ml to obtain herba Portulacae crude extractive solution.
Adding the crude extract of herba Portulacae at flow rate of 0.022BV/min into chromatographic column (3.0 cm × 180 cm) filled with 350ml of polyvinylpyrrolidone for adsorption, eluting with 2.5BV distilled water after sample loading, removing sugar and protein components, eluting with 80% ethanol aqueous solution with volume concentration of 4.5BV, collecting the eluate, and concentrating the eluate on rotary evaporator (0.09MPa, 60 deg.C) under reduced pressure until the water content is less than 5% to obtain about 1.1g of herba Portulacae lactam extract. The total content of the purslane lactam (I and II) is 80.1 percent through liquid phase analysis.
Liquid phase conditions: eclipse SB-C8 column (4.6 mm. Times.250mm, 5 μm); gradient elution conditions of mobile phase mixed solvent A (acetonitrile) and solvent B (0.01% trifluoroacetic acid water, v/v): 40-100% A (0-10 min), 100-40% A (10-16 min), 40% A (16-18 min). Flow rate 1.0 mL/min-1(ii) a The detection wavelength is 210nm; the column temperature is 30 ℃; the amount of the sample was 20. Mu.L.
COMPOUND I R＝H
COMPOUND II R＝OCH3
Compound nuclear magnetic data are shown in table 1 below.
TABLE 1 Compounds I and II1H NMR and13C NMR(600MHz)
example 2
Research on therapeutic effect of purslane lactam extract on monocrotaline-induced pulmonary hypertension rats
Healthy male SD rats (280-300 g) were divided into 60 groups at random: blank control group, model group, positive control group (20 mg/Kg), low, medium and high dose group (50 mg/Kg,100mg/Kg,150 mg/Kg). After adaptive feeding for one week, the rats except the blank control group are all subjected to neck-back subcutaneous injection of 55mg/kg monocrotaline to establish a pulmonary artery high pressure rat Model, administration is started after two weeks, wherein the low, medium and high dose components are respectively administered for continuous intragastric administration for two weeks, and the blank control group and the Model group are administered with equal volume of solvent. Two weeks after administration, pulmonary arterial pressure was measured by right-cardiac catheterization and the model set-up and the effect of the compound on rats with pulmonary hypertension was evaluated.
Right Ventricular Systolic Pressure (RVSP) levels can be used to assess the severity of pulmonary hypertension. The results show that there was a significant reduction in RVSP in rats treated with the positive control group and the high dose group of purslane lactam extract over 20 days after administration.
Mean pulmonary arterial pressure (mPAP) level is one of the important hemodynamic indicators to assess the severity of pulmonary arterial hypertension. After 20 days of administration, the positive drug sildenafil-treated rat mPAP was observed to be significantly lower than the MCT group, and the purslane lactam extract-treated rat mPAP was also significantly decreased compared to the model group.
The results show that the purslane lactam extract can improve the pulmonary hypertension of rats caused by monocrotaline to a certain extent.
Claims (9)
1. The purslane lactam extract is characterized by being prepared by the following method:
(1) Cleaning fresh purslane, drying, crushing and sieving to obtain purslane powder, and extracting with ethanol to obtain an extract;
(2) Dispersing the extract obtained in the step (1) with water, adding chitosan, stirring at room temperature for 2-6 h, then centrifuging, and removing precipitates to obtain a supernatant; adding an extracting agent into the supernatant to obtain a mixed solution, stirring the mixed solution for 30 to 90min at the temperature of between 50 and 80 ℃ for extraction, then cooling the mixed solution to between 30 and 40 ℃, standing and layering the mixed solution to obtain an upper layer of extract liquor and a lower layer of raffinate, and concentrating the upper layer of extract liquor under reduced pressure to obtain a purslane crude extract;
the extractant is formed by mixing an organic solvent A and an organic solvent B according to the volume ratio of 500.5-5, wherein the organic solvent A is a mixed solution of ethyl acetate and n-butanol according to the volume ratio of 1-3:1; the organic solvent B is acetic acid;
(3) Adding the purslane crude extract obtained in the step (2) into a chromatographic column filled with polyvinylpyrrolidone at the speed of 0.02-0.08 BV/min, eluting with 2-5 BV of distilled water until the effluent is colorless, eluting with 70-80% ethanol aqueous solution with the volume concentration of 3-5 BV, collecting the eluent, and removing the solvent by concentration under reduced pressure to obtain the purslane lactam extract.
2. The purslane lactam extract of claim 1, wherein in step (1), the ethanol extraction method comprises: mixing purslane powder with ethanol in a mass ratio of 1:7-9, stirring and soaking for 1-3 h at room temperature, then heating to 70-100 ℃, performing reflux extraction for 0.5-3 h, then cooling to 30-50 ℃, filtering to obtain filtrate, namely the purslane alcohol extract, and concentrating under reduced pressure until no ethanol smell exists to obtain an extract.
3. The purslane lactam extract of claim 1, wherein in step (2), the extract is dispersed in water by 20-30 times the volume of the extract.
4. The purslane lactam extract of claim 1, wherein in step (2), the chitosan is added in an amount of 1/200 to 1/300 of the mass of the purslane powder.
5. The purslane lactam extract of claim 1, wherein in step (2), the volume of the extractant is 10-20 times that of the extract.
6. The purslane lactam extract of claim 1, wherein in step (2), the upper extract is concentrated under reduced pressure to 0.02 to 0.05 times the volume of the mixed solution.
7. The purslane lactam extract of claim 1, wherein in step (3), the column chromatography operation is: adding the purslane crude extract obtained in the step (2) into a chromatographic column filled with polyvinylpyrrolidone at the speed of 0.03-0.05 BV/min, eluting with 2-4 BV of distilled water until the effluent is colorless, eluting with 70-80% ethanol aqueous solution with the volume concentration of 3-4 BV, collecting the eluent, and removing the solvent by concentration under reduced pressure to obtain the purslane lactam extract.
8. The purslane lactam extract of claim 1, wherein the purslane lactam extract has a total of compounds represented by formula I and formula II that account for more than 75% of the total weight of the purslane lactam extract;
9. the use of the purslane lactam extract of claim 1 in the preparation of a medicament for the prevention and treatment of pulmonary hypertension.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102973619A (en) * | 2012-12-31 | 2013-03-20 | 山东大学 | Process for extracting indoline amide alkaloid from purslane and detection methods for indoline amide alkaloid |
| CN112409307A (en) * | 2020-11-26 | 2021-02-26 | 辽宁中医药大学 | Compound Olerafuran A in purslane, and extraction and separation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102973619A (en) * | 2012-12-31 | 2013-03-20 | 山东大学 | Process for extracting indoline amide alkaloid from purslane and detection methods for indoline amide alkaloid |
| CN112409307A (en) * | 2020-11-26 | 2021-02-26 | 辽宁中医药大学 | Compound Olerafuran A in purslane, and extraction and separation method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| TAN YUE ET AL: "The Effects of Portulaca oleracea on Hypoxia-Induced Pulmonary Edema in Mice", 《HIGH ALTITUDE MEDICINE & BIOLOGY》, vol. 16, no. 1, pages 43 - 51 * |
| YAO YAO ET AL.: "Tamaractam, a New Bioactive Lactam from Tamarix ramosissima, Induces Apoptosis in Rheumatoid Arthritis Fibroblast-Like Synoviocytes", 《MOLECULES》, pages 1 - 9 * |
| 徐靓等: "马齿苋醇提物中羟基二氢博伏内酯的分离及结构鉴定", 《辽宁中医杂志》, vol. 44, no. 1, pages 122 - 124 * |
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