CN103239435A - Preparation method of gynura divaricata total caffeoylquinic acid and application in antihyperglycemic agent or health-care product - Google Patents
Preparation method of gynura divaricata total caffeoylquinic acid and application in antihyperglycemic agent or health-care product Download PDFInfo
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Abstract
The invention discloses a preparation method of gynura divaricata total caffeoylquinic acid and application of the gynura divaricata total caffeoylquinic acid in an antihyperglycemic agent or a health-care product. The effective part of the gynura divaricata total caffeoylquinic acid takes an overground part of gynura plant gynura divaricata (gynura divaricata) as a material; the preparation method comprises the steps of refluxing and extracting the dry overground part of the gynura divaricata through certain concentration of ethanol; filtering, concentrating, drying and dissolving by a hydrochloric acid solution; filtering, and extracting filtrate by ethyl acetate, redissolving an ethyl acetate extract through low-concentration ethanol, gradiently eluting by macroporous resin water ethanol, gathering phenolic acid ingredients, and recovering a solvent to dry and obtain the effective part of the total caffeoylquinic acid. The gynura divaricata total caffeoylquinic acid prepared by the method has significant inhibited effect on important target-protein-tyrosine-phosphatase 1B for researching intestinal carbohydrate hydrolase alpha-glucosaccharase and diabetes mellitus, and can be further researched and developed as a drug or a health-care product for auxiliary treatment of the diabetes mellitus. The invention provides a certain scientific basis for civil application of the gynura divaricata for treatment of the diabetes mellitus, and provides a new resource for development of a safe and efficient novel antihyperglycemic agent or health-care product.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to a kind of method and the application of this effective site in treatment diabetes medicament or health product of from the Chinese medicine Gynura divaricata, extracting and preparing total caffeoylquinic acids effective site.
Background technology
Gynura divaricata (Gynura bicolor DC.) belongs to herbaceos perennial for Compositae (Compositae) Radix Gynurae, has another name called Radix et Rhizoma Gynurae divaricatae, mainly is distributed in China's southern area.Gynura divaricata in Jiangsu, Zhejiang, Sichuan and Fujian is among the people, win its fresh blade or with stem and leaf to boil water the taking of making tea, the treatment diabetes had curative effect preferably.Institute of Botany began introducing and planting in 2000, and carried out The Chemical Constituents work at treating diabetes.
Chemical constitution study shows that Gynura divaricata mainly contains the chemical combination composition of other types such as alkaloids, flavonoid, cerebroside, organic acid and adenosine, uridnine.Animal pharmacological test confirms that the water extract of Gynura divaricata has significant hypoglycemic activity (Hu Yong etc., Xi'nan College of Forestry journal, 2007,27 (1): 55-58; Horse due east etc., Radix et Rhizoma Gynurae divaricatae water extract are to hypoglycemic activity and the mechanism thereof of type 2 diabetes mellitus rat, Chinese herbal medicine, and 2010,41 (4), 623-626).The invention disclosed patent 200710084533.2,200610052502.4, and 201110372288.1 point out that all Gynura divaricata has the diabetes effect.
In the clinical treatment of type 2 diabetes mellitus, glycoside hydrolase inhibitor such as alpha-glucosidase, maltase and saccharase inhibitor are a class reaches the treatment diabetes to delay the intestinal carbohydrate absorption orally-taken blood sugar reducing medicines.Because being closely connected of alpha-glucosidase and diabetes, the medicine scholar is devoted to seek the inhibitor of this fermentoid always, to develop more treatment diabetes medicament.At present, come into the market and clinically widely used alpha-glucosidase inhibitor class antidiabetic drug mainly contain: acarbose (acarbose), voglibose (voglibose), miglitol (miglitol) etc.
(protein tyrosine phosphatase-1B PTP1B) is an important target in the diabetes study to PTP 1B.As one of member of typical non-receptor type PTPase family, PTP1B in insulin signaling pathway by negative regulation Insulin receptor INSR (insulin receptor), thereby reach the effect of control blood glucose.Seek the specific inhibitor of PTP1B, improve the sensitivity of insulin signaling pathway by the activity that suppresses PTP1B, treatment of diabetes is had important application prospects.
Summary of the invention
The objective of the invention is to find and the position of the anti-diabetic validation department of the Chinese Academy of Sciences in the Gynura divaricata is provided.
In order to achieve the above object, the invention provides preparation method and the purposes in preparation antidiabetic medicine or health product thereof of the total caffeoylquinic acids of Gynura divaricata.
The total caffeoylquinic acids effective site of Gynura divaricata provided by the invention is raw material with the dry aerial parts of Gynura divaricata, prepares by following operating procedure:
(1) with Gynura divaricata aerial parts drying with after pulverizing, be 60-100% alcoholic solution reflux, extract, with mass percent concentration, 6～10 times of solid-liquid ratios (L/kg), extraction time is 1-3 time, and extracting temperature is 50-80 ℃, and extraction time is 1-3 hour, merge extractive liquid,, filter, filtrate decompression is concentrated into does not have the alcohol flavor, and vacuum drying obtains the crude extract powder.
(2) the described ethanol crude extract of step (1) powder with 2～5% aqueous hydrochloric acid solutions dissolving of certain volume, filters rear filtrate ethyl acetate extraction 2 times earlier, and the combined ethyl acetate layer reclaims solvent, obtains acetic acid ethyl ester extract.
(3) the described acetic acid ethyl ester extract of step (2) redissolves through low-concentration ethanol water again, the macroporous resin column of flowing through D101 absorption, use earlier the deionized water rinsing resin, reuse water-ethanol gradient elution, the collection concentration of alcohol is the eluent between the 40-60%, concentrating under reduced pressure, drying obtains total caffeoylquinic acids effective site.
The total caffeoylquinic acids effective site of Gynura divaricata so that said method prepares comprises following active component: 3,4-O-dicaffeoylquinic acid, 3, the 5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid, 3,4-O-dicaffeoylquinic acid methyl ester, 3,5-O-dicaffeoylquinic acid methyl ester, 4,5-O-dicaffeoylquinic acid methyl ester.Calculate quality percentage composition＞50% of total phenolic acid in this effective site with dry product weight.
The total caffeoylquinic acids effective site of above-mentioned Gynura divaricata has alpha-glucosidase, protein-tyrosine phosphatase 1B inhibitor effect, can be applied to prepare antidiabetic medicine or health product.
Described antidiabetic medicine or health product be respectively contain treatment effective dose or functional component the total caffeoylquinic acids effective site of Gynura divaricata at pharmaceutically acceptable carrier and health food.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1:
Getting Gynura divaricata dry aerial parts 300g, pulverize, is 80% alcoholic solution 3000mL with mass percent concentration 70 ℃ of following reflux, extract, 2 times, and merge extractive liquid, filters, and being evaporated to does not have alcohol and distinguish the flavor of, and vacuum drying obtains the crude extract powder;
With above-mentioned crude extract powder, earlier with 2% aqueous hydrochloric acid solution dissolving of certain volume, filter rear filtrate with 500mL ethyl acetate extraction 2 times, the combined ethyl acetate layer reclaims solvent, obtains ethyl acetate extract.
Take by weighing macroporous adsorbent resin (D101) 600g, the adding distilled water is at room temperature placed and is spent the night, make the abundant swelling of resin, wet method dress post, flow cleaning pillar to effluent and the volume ratio of water with 95% ethanol is the muddiness that is not white in color when mixing at 1: 5, do not have the ethanol flavor with the abundant drip washing pillar of distilled water to effluent then, placement is spent the night;
Above-mentioned ethyl acetate extract dissolves through 10% ethanol water (v/v), filter, filtrate is slowly flow through the macroporous resin column that above-mentioned processing and balance are crossed, use earlier deionized water rinsing, reuse Different concentrations of alcohol gradient elution, the collection concentration of alcohol is the eluent between the 40-60%, and effluent launches through TLC, sprays 5% FeCl
3Alcoholic solution shows aeruginous; Concentrating under reduced pressure is collected liquid, and lyophilization obtains total caffeoylquinic acids effective site.Calculate quality percentage composition＞50% of total phenolic acid in this position with dry product weight.
The total caffeoylquinic acids effective site that more than obtains certain volume chromatographically pure dissolve with methanol, 45 μ m filtering with microporous membranes are prepared type high performance liquid chromatography (Agilent Prep-HPLC1100) and separate, and chromatographic process is as follows:
Mobile phase: A water (0.1% formic acid), B acetonitrile; Elution process: isocratic elution, 20%B, 0-30mmin; Linear elution, 20-30%B, 30-55min; Linear elution 30-20%, 55-57min; Flow velocity 6mL/min, room temperature detects wavelength 325nm, the each 250 μ L of sampling volume, running time 57mins, C18 post (21.2mm ID * 150mm, 5 μ m) separates, automatic fraction collector peak trigger mode is collected fraction.
Collect fraction respectively, concentrating under reduced pressure and through high vacuum dry obtains 6 coffee mesitoyl quinine acid compounds, according to MS and NMR data and document comparison, identify that their structure is respectively: 3,4-O-dicaffeoylquinic acid (1), 3,5-O-dicaffeoylquinic acid (2), 4,5-O-dicaffeoylquinic acid (3), 3,4-O-dicaffeoylquinic acid methyl ester (4), 3,5-O-dicaffeoylquinic acid methyl ester (5), 4,5-O-dicaffeoylquinic acid methyl ester (6); Except chemical compound 3, outside the 5-O-dicaffeoylquinic acid (2), other 5 coffeic acyl quininic acid derivatives are to separate from Gynura divaricata first and obtain.The structure of each chemical compound is as follows:
Embodiment 2: total phenolic content of the total caffeoylquinic acids effective site of Gynura divaricata is measured (colorimetry)
With 3, (the self-control of 4-O-dicaffeoylquinic acid, HPLC detects its purity＞95%) be reference substance bioassay standard curve, standard substance are dissolved in acetone-water solution are made into series concentration, in the 10mL volumetric flask, add the 8mL reference substance solution, add Folin-Ciocalteau reagent 0.5mL, shake up, place 1min.Add 20%Na again
2SO
4Solution 1.5mL shakes up, and places 1h, measures trap, drawing standard curve at the 750nm place in spectrophotometer.
Accurately take by weighing the total caffeoylquinic acids effective site of Gynura divaricata sample, as stated above, in 750nm place working sample trap.Calculate according to standard curve, in the total caffeoylquinic acids effective site of Gynura divaricata, with 3,4-O-dicaffeoylquinic acid meter, quality percentage composition＞50% of total phenolic acid.
Embodiment 3: the external hypoglycemic activity of the total caffeoylquinic acids effective site of Gynura divaricata and coffeic acyl quininic acid derivative thereof is measured
(1) inhibition of alpha-glucosidase is tested
Alpha-glucosidase (α-glucosidase, Type I) is purchased the company in sigma, Infinite F50 type microplate reader (Tecan, Switzerland); Each monomeric compound sample takes out a certain amount of respectively, is dissolved in the pure methanol, and being made into concentration is the high concentration mother solution of 100mg/mL; Adopt 96 orifice plates screening system, reaction system reference literature reported method, do change slightly, reaction system after improving and optimizating is: 28 μ L phosphate buffer (phosphate buffer, PBS, pH=6.8) add alpha-glucosidase (1U/mL) 10 μ L in, add certain density sample solution 2 μ L, 37 ℃ of constant temperature 10min, add then nitre phenyl-β-D-pyranglucoside (4-nitrophenyl β-D-glucopyranoside, PNPG, 10mM in PBS) 10 μ L, 37 ℃ of isothermal reaction 35min measure absorbance (A value) under the 405nm wavelength.Acarbose (acarbose, acarbose) purchases white Bayer A.G, positive control for this law, set blank (only with buffer) and negative control (only with buffer and enzyme liquid) simultaneously, the enzymatic activity suppression ratio is calculated as follows: and the enzymatic activity suppression ratio (Inhibitory, %)=(A negative control-A sample)/(A negative control-A blank) * 100%.Positive control medicine acarbose (acarbose).As calculated, the IC of the right alpha-glucosidase of positive control acarbose
50Be 1.38mM.
(2) inhibition of protein tyrosine phosphatase esterase 1B is tested
The PTP1B enzyme is mixed with the methanol solution of 10mg/mL available from Enzo Life Science company after all chemical compound weighings, add 2 μ l and do not influence enzymatic activity in every hole.Adopt the screening of 96 orifice plates, reaction system reference literature reported method, do change slightly, add following reagent and be mixed with the reaction solution of 100 μ L: 0.05 μ g PTP1B enzyme, 1.5mM Insulin receptor INSR β residues (IR5) and 100mM MES buffer (300mM sodium chloride, 2mM EDTA, 2mM DTT, 0.1%NP-40, pH=6.0); Be incubated 30min down at 37 ℃, use certain density phosphate detectable (available from Enzo Life Science company) end reaction at last, change (Infinite F50 microplate reader, Switzerland Tecan company) by measuring its absorption value at the 620nm place, calculate its suppression ratio.Suppression ratio is calculated as follows: [1-(Asample/Acontrol)] * 100%.Adopt PTP1B enzyme inhibitor SURAMIN (purchase white Enzo Life Sciences company) as positive control.
The compound monomer composition that the total caffeoylquinic acids effective site of Gynura divaricata and wherein separating obtains to the inhibition activity of alpha-glucosidase and protein tyrosine phosphatase esterase 1B see Table 1, table 2.
Table 1 sample is to the inhibition activity of alpha-glucosidase
Table 2 sample is to the inhibition activity of protein tyrosine phosphatase esterase 1B
External alpha-glucosidase activity is measured and is found: the total caffeoylquinic acids effective site of Gynura divaricata with therefrom separate the di-coffee mesitoyl quinine acid compounds monomer that obtains especially 3,4-O-dicaffeoylquinic acid methyl ester and 4,5-O-dicaffeoylquinic acid methyl ester has all shown significant alpha-glucosidase and has suppressed active, their IC
50Value all significantly is lower than positive control medicine acarbose.External protein tyrosine phosphatase esterase 1B determination of activity is found: the total caffeoylquinic acids effective site of Gynura divaricata and 3,5-O-dicaffeoylquinic acid and 4,5-O-dicaffeoylquinic acid monomer have showed stronger protein tyrosine phosphatase esterase 1B and have suppressed active.Infer that thus coffee mesitoyl quinine acid compounds is the hypoglycemic active substance of Gynura divaricata basis, for the application among the people of illustrating Gynura divaricata treatment diabetes provides scientific basis.
Above-described embodiment is preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification made under essence of the present invention and the principle, substitutes, combination and simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. the preparation method of the total caffeoylquinic acids of Gynura divaricata and the application in antidiabetic medicine or health product thereof, the preparation method that it is characterized in that the total caffeoylquinic acids of Gynura divaricata comprises following operating procedure: with Gynura divaricata aerial parts drying with after pulverizing, with the alcoholic solution reflux, extract,, extracting liquid filtering, being evaporated to does not have the alcohol flavor, and vacuum drying obtains the crude extract powder.The crude extract powder dissolves through aqueous hydrochloric acid solution, and filtrate is used ethyl acetate extraction, again through macroporous resin adsorption, and the water-ethanol gradient elution, eluent is concentrated, dry.The purposes of the total caffeoylquinic acids of Gynura divaricata comprise its antidiabetic medicine or (with) application in the health product.
2. Gynura divaricata according to claim 1 is slightly got thing, it is characterized in that: the mass percent concentration of described alcoholic solution is 60-100%, and consumption is 6-10 times of quality of medicinal material volume, and extraction time is 1-3 time, extracting temperature is 50-80 ℃, and extraction time is 1-3 hour.
3. the preparation method of the total caffeoylquinic acids of Gynura divaricata according to claim 1, it is characterized in that: described through the extraction of finite concentration alcoholic solution and the dry crude extract powder that obtains, 2～5% aqueous hydrochloric acid solutions with certain volume dissolve earlier, filter, filtrate is used ethyl acetate extraction 2 times, the combined ethyl acetate layer reclaims solvent, obtains ethyl acetate extract; Redissolve through low-concentration ethanol water, the deionized water rinsing resin is used earlier in the macroporous resin column of flowing through D101 absorption again, reuse water-ethanol gradient elution, collection concentration of alcohol are the eluent between the 40-60%, concentrating under reduced pressure, drying obtains total caffeoylquinic acids effective site.
4. the total caffeoylquinic acids effective site that obtains according to claim 2 and 3 described methods is characterized in that this effective site comprises following active component: 3,4-O-dicaffeoylquinic acid, 3, the 5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid, 3,4-O-dicaffeoylquinic acid methyl ester, 3,5-O-dicaffeoylquinic acid methyl ester, 4,5-O-dicaffeoylquinic acid methyl ester.
5. the total caffeoylquinic acids effective site of Gynura divaricata according to claim 4, it is characterized in that: the dry product weight with the total caffeoylquinic acids effective site of Gynura divaricata is calculated quality percentage composition＞50% of the total phenolic acid of the total caffeoylquinic acids effective site of Gynura divaricata.
6. suppress alpha-glucosidase, the antidiabetic medicine of PTP 1B or the application on the health product according to claim 1,4, the total caffeoylquinic acids effective site of 5 described Gynura divaricatas in preparation.
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| CN108239096B (en) * | 2016-12-26 | 2021-01-12 | 中国医学科学院药物研究所 | Chrysanthemum morifolium extract compound, pharmaceutical composition thereof and application of chrysanthemum morifolium extract compound in preventing and treating neurodegenerative diseases |
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