CN101185665A - Method for preparing total flavone of bidens bipinnata - Google Patents
Method for preparing total flavone of bidens bipinnata Download PDFInfo
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Abstract
The invention discloses a preparation method of spanishneedles herb total flavonoids, which can be obtained by the following steps: the spanishneedles herb is extracted through ethanol reflux; minimum quantity of ethanol is recovered, impurities are removed by standing and organic solvent is used for defatting; then mixed solvent is extracted beneficiation and resin purification, thus spanishneedles herb total flavonoids is obtained. The obtained flavone extract has high flavone content, over 50%. With simple and feasible technique, and high extract yield rate, the invention is suitable for industrialized production. The total flavonoid extract obtained from the invention has the effect of reducing blood pressure, blood lipid and blood sugar, anti-oxidation and preventing hepatic fibrosis, which can prepare drugs for treating cardiovascular diseases, reducing blood pressure, blood lipid and blood sugar as well as preventing haptic fibrosis.
Description
Technical field
The present invention relates to a kind of preparation method of Herba Bidentis Bipinnatae active component, belong to natural drug active component preparation field.
Background technology
Bidens Compositae (Compositae) Bidens plant, have another name called Herba Bidentis Bipinnatae, terrible hairpin grass, Herba Bidentis Bipinnatae, lead-in wire bag, pin bag grass, pin, bean dregs dish, Herba silenes fortunei, originate in ground such as northeast, North China, East China, southwest and Shaanxi, Gansu, grow in roadside, wasteland, hillside and field." Chinese medicine voluminous dictionary " record " the Herba Bidentis Bipinnatae bitter in the mouth is flat, and nontoxic, the merit of heat-clearing and toxic substances removing, dissipating blood stasis for subsidence of swelling cures mainly malaria, diarrhoea, dysentery, hepatitis acute nephritis, stomachache, acute appendicitis, laryngopharynx swelling and pain, traumatic injury, snake bite and insect sting etc. ".Herba Bidentis Bipinnatae can be used for treating flu, goiter, chronic pelvic inflammatory disease, uterine prolapse, neurasthenia etc. better curative effect; Its preparation is pleased a year sheet has better curative effect to essential hypertension; Diabetes are treated with its water decoction in the Yunnan Province of China minority area, and as seen this plant has higher medicinal exploitation value.In recent years, pharmacological action to Herba Bidentis Bipinnatae flavone and liposoluble ingredient has more research, liposoluble ingredient in the Herba bidentis parviflorae, be mainly quinic acid, caffeic acid, protocatechuic acid, the calculation of hydroxyl Cortex cinnamomi japonici (Ramulus Cinnamomi), caffeoylquinic acids etc. had the effect (Wang Jue that suppresses histamine release, Wang Naili, Deng. liposoluble ingredient and inhibition histamine releasing activity thereof in the Herba bidentis parviflorae. Chinese pharmaceutical chemistry magazine [J] .2006,16 (3): 168).The document record, Sticktight general flavone has the Fibrotic effect of Chinese People's Anti-Japanese Military and Political College's Hepar Mus, and the effect that has blood pressure lowering, transfers blood fat.(Li Shuai such as Li Shuai, Kuang Haixue, Kuang Haixue, Deng. Herba Bidentis Bipinnatae extract is to the research of type ii diabetes mice hypoglycemic activity. Chinese medicine journal [J] 2003,31 (5): 37) Herba Bidentis Bipinnatae normal hexane, ethyl acetate, n-butyl alcohol extract, water extract part are carried out hypoglycemic activity research to the type ii diabetes mice, find that ethyl acetate, n-butanol extraction position can reduce the blood glucose of normal mouse.The disclosed Herba Bidentis Bipinnatae extract of Chinese patent CN1899340A (mainly containing total flavonoid and two caffeoyl compounds) has hypoglycemic activity.
Herba Bidentis Bipinnatae contains multiple bioactive ingredients, is its main component with flavone compound wherein, also has phenolic acids, volatile oil, amino acids, triterpene and steroidal class, a small amount of alkaloid compound in addition.The contained flavone amount of the different medicinal parts of Herba Bidentis Bipinnatae difference is bigger, document (Feng Qiang. Herba Bidentis Bipinnatae different parts general flavone content colorimetry is relatively. and modern Chinese medicine is studied and is put into practice [J] .2003,17 (2): 25) report, Herba Bidentis Bipinnatae herb total flavonoids content is 5.40%, the blade general flavone content is 6.66%, and the inflorescence general flavone content is 6.68%, and stem leaf total flavones content is 0.89%, general flavone content is 3.24% in the fruit, and is the highest with content in blade and the inflorescence.
Technical study to Sticktight general flavone, so that more bibliographical information to be arranged, wherein mostly is to be the enrichment carrier with the macroporous adsorbent resin, research emphasis lays particular emphasis on the investigation of the macroporous adsorbent resin of different model to the adsorbance and the elution amount of Sticktight general flavone, and wherein mostly is to directly investigating with the extracting solution behind the ethanol extraction, and such processing has strengthened the load of macroporous resin.As document (1, Wei Yingqin, Ma Yi etc. the research of macroporous adsorbent resin separation and purification Sticktight general flavone. the time precious traditional Chinese medical science traditional Chinese medicines [J] .2006,17 (11): 2257-2258; 2, clock is bright and beautiful, Chen Feihu etc. the Study on extraction of total flavones in the preferred Herba Bidentis Bipinnatae of orthogonal design. the time precious traditional Chinese medical science traditional Chinese medicines [J] .2006,17 (12): 2520-2521), these methods are too easy when handling crude drug, resulting product general flavone content is relatively low, impurity content is also higher relatively, and excessive to the load capacity of resin, and resin demand is too much.Chinese patent CN1899340A discloses a kind of method that obtains Sticktight general flavone, its used method is that Herba Bidentis Bipinnatae ethanol percolation liquid concentrates after defat with petroleum ether, ethyl acetate extraction promptly gets the total flavones activity extract, but its efficiency of pcr product is low, end product is 40g in the dry Herba Bidentis Bipinnatae medical material of 10kg, and the significant loss degree is big.
Summary of the invention
The object of the present invention is to provide the preparation method of the higher and Sticktight general flavone that the Sticktight general flavone efficiency of pcr product is high of a kind of content.
The present invention is a raw material with the medical material Herba Bidentis Bipinnatae, and wherein Herba Bidentis Bipinnatae can be Herba Bidentis Bipinnatae blade, inflorescence, herb or fruit.
Among the present invention, Herba Bidentis Bipinnatae is earlier with 60%～90% alcohol reflux, the gained ethanol extract is after decompression recycling ethanol to ethanol content is lower than 15%, liquor strength is about every milliliter and contains crude drug 0.7～0.85g, medicinal liquid after reclaiming is put cold place to be placed 24 hours, separate out insoluble matter in the medicinal liquid, filtration or centrifugal, insoluble matter discards, clear liquid is removed ethanol, and with low polar organic solvent extraction defat, medicinal liquid reuse after the defat and the immiscible organic solvent extraction of water are with the flavone compound in the preliminary enrichment medicinal liquid, with the concentrated used organic solvent of extraction of removing of the flavonoid medicinal liquid of enrichment, the concentrated solution thin up of gained disperses after resin treatment, with Different concentrations of alcohol eluting resin column, collection contains stream part of flavonoid, promptly gets the Sticktight general flavone extract.Its general flavone content is more than or equal to 50%.
Among the present invention, the extraction process of Herba Bidentis Bipinnatae can be specially: Herba Bidentis Bipinnatae is earlier with 60%～90% alcohol reflux, the gained ethanol extract is after decompression recycling ethanol to ethanol content is about 10%, liquor strength is about every milliliter and contains crude drug 0.80g, medicinal liquid after reclaiming is put cold place to be placed 24 hours, separate out insoluble matter in the medicinal liquid, filtration or centrifugal, insoluble matter discards, clear liquid is with the n-hexane extraction defat, and 4: 1 n-butyl alcohol of the medicinal liquid reuse after the defat-ethyl acetate mixed extractant solvent is with the flavone compound in the preliminary enrichment medicinal liquid, with the concentrated used organic solvent of extraction of removing of the flavonoid medicinal liquid of enrichment, the concentrated solution of gained adds the suitable quantity of water dilution, disperse after macroporous adsorptive resins is handled, resin is used 3～5 column volumes of deionized water eluting earlier, reacts to Molish and is negative, use 50%～80% ethanol elution instead, collect ethanol elution, concentrating under reduced pressure, drying, pulverize, promptly get Sticktight general flavone extract dried cream powder.Its general flavone content is more than or equal to 50%.
Particularly, the extraction process of Sticktight general flavone of the present invention can also be: Herba Bidentis Bipinnatae is earlier with 60%～90% alcohol reflux, the gained ethanol extract is after decompression recycling ethanol to ethanol content is about 10%, liquor strength is about every milliliter and contains crude drug 0.80g, medicinal liquid after reclaiming is put cold place to be placed 24 hours, separate out insoluble matter in the medicinal liquid, filtration or centrifugal, insoluble matter discards, clear liquid is with the petroleum ether extraction defat, and 4: 1 n-butyl alcohol of the medicinal liquid reuse after the defat-ethyl acetate mixed extractant solvent is with the flavone compound in the preliminary enrichment medicinal liquid, with the concentrated used organic solvent of extraction of removing of the flavonoid medicinal liquid of enrichment, the concentrated solution of gained adds the appropriate amount of deionized water dilution, disperse after polyamide resin column is handled, resin is used 3～5 column volumes of deionized water eluting earlier, reacts to Molish and is negative, use 50%～80% ethanol elution instead, collect ethanol elution, concentrating under reduced pressure, drying, pulverize, promptly get Sticktight general flavone extract dried cream powder.Its general flavone content is more than or equal to 50%.
Among the present invention, the used extractant of preliminary enrichment Sticktight general flavone is except being n-butyl alcohol-ethyl acetate mixed solvent of 4: 1, it can also be single n-butyl alcohol of using, or single ethyl acetate of using, or with other ratio of n-butyl alcohol and ethyl acetate mixed solvent, its used solvent is all saturated in advance through water.
Among the present invention, before using resin treatment, the Herba Bidentis Bipinnatae medicinal liquid that contains flavone is handled through extraction, remove impurity, defat, preliminary enrichment, make other impurity constituents in the medicinal liquid significantly reduce, the composition of flavonoid is also relatively higher and pure, so not only alleviated the load of resin, and the direct upper prop processing of medicinal liquid that consumption was not also handled is few, the product content of total flavone that obtains also is improved.
In the treatment process process of the present invention, also can in remove impurity, two step of defat program, singly use a kind of program, promptly after the concentrating and precipitating remove impurity, do not adopt low polar organic solvent extraction, directly enter into ethyl acetate or normal hexane or n-butyl alcohol-ethyl acetate mixed extractant solvent process; Perhaps do not adopt the precipitation remove impurity, be concentrated into and contain ethanol and be lower than 15% back and directly adopt normal hexane or petroleum ether extraction defat, then with ethyl acetate or n-butyl alcohol or n-butyl alcohol-ethyl acetate mixture extraction process; Among the present invention, treatment process can also be the Herba Bidentis Bipinnatae medical material through extracting, and the medicinal liquid behind the condensed skimmed is directly gone up the resin column processing, and saves ethyl acetate or n-butyl alcohol or n-butyl alcohol-ethyl acetate mixed extractant solvent process; Or the Herba Bidentis Bipinnatae medical material is after extract, be concentrated into to contain and leave standstill remove impurity after amount of alcohol is lower than 15%, the last clear liquid medicine after the remove impurity boils off remaining ethanol again, last resin column processing.Last processing procedure also all drops within protection scope of the present invention.But the medicinal liquid before the last processing method gained upper prop is pure, impure also many than preceding method not as preceding method.
Gained Sticktight general flavone extract of the present invention, have blood pressure lowering, blood fat reducing, blood sugar lowering, antioxidation, prevent the effect of hepatic fibrosis, can be used for preparing the medicine that has the effect of treatment cardiovascular disease, blood pressure lowering, blood fat reducing, blood sugar lowering and prevent hepatic fibrosis.
Below from pharmacological evaluation effect of the present invention is described, but for pharmacology embodiment and be confined to this effect, and be a kind of nonrestrictive explanation.
Blood pressure lowering experiment to the irritability Hypertensive Rats
The Wistar rat adapted to for 1 week in specified environment after, put it in the different-style of MG-2 type labyrinth stimulator, with the discontinuity alternating current, intensity 2-4mA, persistent period is 50ms, the interval of each energising is controlled by computer program, 2 the random time length of electric shock interval between 3-30s, the output of electric current is irregular to follow, stress intensity thereby strengthened, make it to produce the anxiety on the highly spirit and emotion, increase psychentonia stimulates in order to reduce the corporality noxious stimulus more, follow a noise signal (80～100ds, time-histories 50ms) setting up trained reflex when shocking by electricity, stressed animal every day stress 2 times, the morning and afternoon each 1 time, each 2h, 2 minor ticks be more than 4 hours, continuously stress 15d, normally feed for drinking water with 2%NaCl solution, and the observation blood pressure, treat that blood pressure on average raises more than the 2.0kPa, be considered as the modeling success.
The Wistar rat of 40 modeling successes is equally divided into 5 groups, model group at random; Verapamil hydrochloride injection (Ver) 12.25mg/kg dosed administration group; Sticktight general flavone extract 20,40,3 dosage groups of 60mg/kg, 8 rats of not modeling are made as blank group (Sham), are left intact, three flavor hypertension pills are respectively organized rat and are irritated stomach 1 time every day, continuous 15 days, model group gave the 10mL/kg normal saline and irritates stomach.Blood pressure lowering the results are shown in Table 1
Table 1 Sticktight general flavone is to the blood pressure lowering influence of irritability Hypertensive Rats
| Group | Dosage | n | 0d p(BP)/kPa | 15d p(BP)/kPa |
| Dosage high dose Ver in the blank model low dosage | - 10mL/kg 20mg/kg 40mg/kg 60mg/kg 12..25mg/kg | 8 8 8 8 8 8 | 15.18±0.51 15.32±0.62 15.04±0.56 15.61±1.12 15.19±0.91 14.96±1.32 | 15.07±0.94 22.45±1.13 19.05±0.97 * 18.54±0.83 ** 17.97±0.62 ** 16.99±1.01 ** |
Compare with model group,
*P＜0.05,
*P＜0.01
By last table result as can be known, each stress rats stress the back mean arterial pressure with stress before compare, blood pressure significantly raises.When giving the animal stress stimulation, rat the lines of strain and fear, accelerated breathing occur, scream, trembles, uprightly, behavior performance such as escape.Behind the gastric infusion 15d, mean arterial pressure is elevated to (22.45 ± 1.13) kPa after the Control group stress in rats, with stress before rat blood pressure relatively, hypertension is remarkable.Mean arterial pressure is (17.97 ± 0.62) kPa after the Sticktight general flavone 60mg/kg group stress in rats, obviously reduce than mean arterial pressure rising range value after the model group stress in rats, P＜0.01, three dosage groups of Sticktight general flavone than the model group stress in rats after mean arterial pressure rising range value remarkable reduction is all arranged, and become dose-dependence.
Influence experiment to the rat fat level
The wistar rat that is 220-250g to 30 body weight is divided into 5 groups at random, establishes 1 blank group, 1 experiment contrast group, 3 experimental grouies respectively.The high lipid food that blank group (A group) feeding standard normal feedstuff, experiment contrast group (B group) are fed and be made up of 1% cholesterol, 10% leaf fat, 0.2% propylthiouracil and 88.8% normal feedstuff; Experimental group is in the high lipid food of feeding, each organizes respectively, and lumbar injection gives Sticktight general flavone 10,15, three dosage groups of 20mg/kg, 6 all posterior veins are got blood, adopt elisa reagent (box) to use the content of the semi-automatic analysis-e/or determining triglyceride (TG) of Vitalab Micro, cholesterol (TC) and high density lipoprotein (HDL-C), go out (LDL-C) according to measurement result calculating low density lipoprotein, LDL sub-thread and reach
LDL-C/HDL-C, HDL-C/TC value the results are shown in Table 1
The influence of table 1 pair rat fat level (
N=6)
| Group | TG /mmol.L-1 | TC /mmol.L-1 | HDL-C /mmol.L-1 | LDL-C /mmol.L-1 | LDL-C/HDL-C | HDL-C/TC |
| A B C D E | 1.50±0.21 2.29±0.22 * 1.26±0.29 **# 1.34±0.31 **# 1.10±0.27 **# | 1.81±0.40 3.71±0.51 * 1.49±0.46 **# 1.57±0.52 **# 1.27±0.40 **# | 1.51±0.49 0.83±0.14 *2.04±0.37 **# 1.93±0.32 **# 2.31±0.27 **# | 0.56±0.24 0.87±0.17 *0.43±0.21 **# 0.48±0.27 **# 0.36±0.31 **# | 0.37±0.16 1.05±0.23 *0.21±0.19 **# 0.25±0.14 **# 0.16±0.20 **# | 0.83±0.42 0.22±0.39 *1.37±0.58 **# 1.23±0.51 **# 1.82±0.49 **# |
Compare with the blank group,
*P＜0.01,
*P＜0.05; Compare with the experiment contrast group,
#P＜0.01
Experimental result shows, the matched group of high lipid food of feeding is compared with the normal control group, TG, TC, LDL-C content, LDL-C/HDL-C obviously improve (P＜0.01) in 6 all backs serum, each experimental group is compared with the blank group, TG, TC, HDL-C level all decrease, and the HDL-C level rises to some extent; Experimental group is compared with the experiment contrast group, and all there were significant differences than the experiment contrast group for every index, illustrates that Sticktight general flavone has the effect that reduces the rat fat level.
Specific embodiment
Embodiment 1
Dry spanishneedles herb leaf 10kg, with 10 times of amount alcohol reflux of 70% 3 times, each 1.5h filters, merging filtrate, filtrate decompression concentrates, and contains amount of alcohol to the medicinal liquid and is about 10%, and liquor strength is about every milliliter and contains Herba Bidentis Bipinnatae blade 0.8g, 24h is placed at cold place, separate out not tolerantly, centrifugal, abandon precipitation, supernatant is with normal hexane (1/2 medicine liquid volume * 3 time) extraction defat, the medicinal liquid concentrating under reduced pressure, remove remaining organic solvent after, the n-butyl alcohol of 4: 1 water saturation of reuse-ethyl acetate mixed extractant solvent, thin out to the extract color, merge mixed extractant solvent liquid, concentrating under reduced pressure removes and desolvates, and concentrated solution disperses with a small amount of distilled water, on the NKA-9 type macroporous adsorptive resins handled well, 4 column volumes of elder generation's water eluting are used 6 column volumes of ethanol elution of 50% instead, collect 50% ethanol elution, concentrate, vacuum drying is pulverized, and gets Sticktight general flavone extract dried cream powder 289g.Measure through ultraviolet visible spectrophotometry, general flavone content is 59%.
Embodiment 2
Herba Bidentis Bipinnatae herb 10kg, with 8 times of amount alcohol reflux of 60% 3 times, each 1h filters, merging filtrate, filtrate decompression concentrates, and contains amount of alcohol to the medicinal liquid and is about 15%, and liquor strength is about every milliliter and contains Herba Bidentis Bipinnatae herb 0.85g, 24h is placed at cold place, separate out not tolerantly, centrifugal, abandon precipitation, supernatant is with normal hexane (1/2 medicine liquid volume * 3 time) extraction defat, the medicinal liquid concentrating under reduced pressure, remove remaining organic solvent after, the n-butanol extraction of reuse water saturation, thin out to the extract color, merge butanol extraction liquid, concentrating under reduced pressure removes and desolvates, and concentrated solution disperses with a small amount of distilled water, on the HP-20 type macroporous adsorptive resins handled well, 3 column volumes of elder generation's water eluting are used 6 column volumes of ethanol elution of 60% instead, collect 60% ethanol elution, concentrate, vacuum drying is pulverized, and gets Sticktight general flavone extract dried cream powder 260g.Measure through ultraviolet visible spectrophotometry, general flavone content is 62%.
Embodiment 3
The dry herb 10kg of Herba Bidentis Bipinnatae, with 10 times of amount alcohol reflux of 80% 3 times, each 1.5h filters, merging filtrate, filtrate decompression concentrates, and contains amount of alcohol to the medicinal liquid and is about 5%, and liquor strength is about every milliliter and contains Herba Bidentis Bipinnatae herb 0.70g, 24h is placed at cold place, separate out not tolerantly, centrifugal, abandon precipitation, supernatant is with petroleum ether (1/2 medicine liquid volume * 3 time) extraction defat, the medicinal liquid concentrating under reduced pressure, remove remaining organic solvent after, the n-butyl alcohol of 4: 1 water saturation of reuse-ethyl acetate mixed extractant solvent, thin out to the extract color, merge mixed extractant solvent liquid, concentrating under reduced pressure removes and desolvates, and concentrated solution disperses with a small amount of distilled water, on polyamide (30-60 order) adsorption resin column handled well, 5 column volumes of elder generation's water eluting are used 6 column volumes of ethanol elution of 70% instead, collect 70% ethanol elution, concentrate, spray drying is pulverized, and gets Sticktight general flavone extract dried cream powder 218g.Measure through ultraviolet visible spectrophotometry, general flavone content is 72%.
Embodiment 4
The Herba Bidentis Bipinnatae dried leaves, with 12 times of amount alcohol reflux of 80% 3 times, each 1.5h filters, merging filtrate, filtrate decompression concentrates, and contains amount of alcohol to the medicinal liquid and is about 8%, and liquor strength is about every milliliter and contains spanishneedles herb leaf 0.75g, 24h is placed at cold place, separate out not tolerantly, centrifugal, abandon precipitation, supernatant is with petroleum ether (1/2 medicine liquid volume * 3 time) extraction defat, the medicinal liquid concentrating under reduced pressure, remove remaining organic solvent after, the extraction of reuse water saturation peracetic acid acetate mixed solvent, thin out to the extract color, the combined ethyl acetate extract, concentrating under reduced pressure removes and desolvates, and concentrated solution disperses with a small amount of distilled water, on polyamide (30-60 order) adsorption resin column handled well, 5 column volumes of elder generation's water eluting are used 6 column volumes of ethanol elution of 80% instead, collect 80% ethanol elution, concentrate, vacuum drying is pulverized, and gets Sticktight general flavone extract dried cream powder 75g.Measure through ultraviolet visible spectrophotometry, general flavone content is 85%.
Embodiment 5
Dry spanishneedles herb leaf 10kg, with the alcohol reflux of 10 times of amounts 70% 3 times, each 1.5h, filter, merging filtrate, filtrate decompression concentrates, contain amount of alcohol to the medicinal liquid and be about 10%, liquor strength is about every milliliter and contains Herba Bidentis Bipinnatae blade 0.8g, and 24h is placed at cold place, separate out not tolerant, centrifugal, abandon precipitation, last clear liquid medicine concentrating under reduced pressure, remove remaining ethanol, the n-butyl alcohol of 4: 1 water saturation of reuse-ethyl acetate mixed extractant solvent, thin out to the extract color, merge mixed extractant solvent liquid, concentrating under reduced pressure removes and desolvates, concentrated solution disperses with a small amount of distilled water, on the NKA-9 type macroporous adsorptive resins handled well, 4 column volumes of first water eluting, use 6 column volumes of ethanol elution of 50% instead, collect 50% ethanol elution, concentrate vacuum drying, pulverize, get Sticktight general flavone extract dried cream powder 294g.Measure through ultraviolet visible spectrophotometry, general flavone content is 52%.
Embodiment 6
The dry herb 10kg of Herba Bidentis Bipinnatae, with 10 times of amount alcohol reflux of 80% 3 times, each 1.5h, filter, merging filtrate, filtrate decompression concentrates, and contains amount of alcohol to the medicinal liquid and is about 5%, and liquor strength is about every milliliter and contains Herba Bidentis Bipinnatae herb 0.70g, concentrated solution is with petroleum ether (1/2 medicine liquid volume * 5 time) extraction defat, the medicinal liquid concentrating under reduced pressure, remove remaining organic solvent after, the n-butyl alcohol of 4: 1 water saturation of reuse-ethyl acetate mixed extractant solvent, thin out to the extract color, merge mixed extractant solvent liquid, concentrating under reduced pressure removes and desolvates, and concentrated solution disperses with a small amount of distilled water, on polyamide (30-60 order) adsorption resin column handled well, 5 column volumes of elder generation's water eluting are used 6 column volumes of ethanol elution of 70% instead, collect 70% ethanol elution, concentrate, spray drying is pulverized, and gets Sticktight general flavone extract dried cream powder 242g.Measure through ultraviolet visible spectrophotometry, general flavone content is 68%.
Embodiment 7
Herba Bidentis Bipinnatae herb 10kg, with 8 times of amount alcohol reflux of 60% 3 times, each 1h, filter, merging filtrate, filtrate decompression concentrate, and contain amount of alcohol to the medicinal liquid and are about 15%, liquor strength is about every milliliter and contains Herba Bidentis Bipinnatae herb 0.85g, 24h is placed at cold place, separates out not tolerant, centrifugal, abandon precipitation, after the supernatant concentrating under reduced pressure is removed remaining ethanol, on the HP-20 type macroporous adsorptive resins handled well, 3 column volumes of first water eluting, use 6 column volumes of ethanol elution of 60% instead, collect 60% ethanol elution, concentrate vacuum drying, pulverize, get Sticktight general flavone extract dried cream powder 313g.Measure through ultraviolet visible spectrophotometry, general flavone content is 51%.
Claims (6)
1. the preparation method of a Sticktight general flavone, it is characterized in that Herba Bidentis Bipinnatae is with 60%～90% alcohol reflux, extracting solution reclaims ethanol and is lower than 15% to containing amount of alcohol, leave standstill remove impurity, after clear liquid extracts defat with low polar organic solvent, continuation with the immiscible middle polarity organic solvent extraction of water enrichment flavone, gained extract decompression is removed behind the extractant with resin purification, the different concentration ethanol eluting, stream part that flavone is rich in collection promptly gets Sticktight general flavone, and the gained general flavone content is more than or equal to 50%.
2. preparation method as claimed in claim 1, it is characterized in that Herba Bidentis Bipinnatae is with 60%～90% alcohol reflux, extracting solution reclaims ethanol and makes and contain amount of alcohol and be lower than 15%, placed 24 hours at cold place, separate out insoluble matter, centrifugal or filter, clear liquid with the n-hexane extraction defat after, continue thin out to the extract color with n-butyl alcohol-ethyl acetate mixed extractant solvent of 4: 1, the enrichment flavone, concentrating under reduced pressure, remove the hybrid extraction solvent after, the concentrated solution thin up, on the macroporous adsorptive resins handled well, first water is eluted to the Molish reaction and is negative, and continues the ethanol elution with 50%～80%, collect ethanol elution, concentrating under reduced pressure, drying is pulverized, get the Sticktight general flavone dry extract, wherein extract obtained general flavone content is more than or equal to 50%.
3. preparation method as claimed in claim 1, it is characterized in that Herba Bidentis Bipinnatae is with 60%～90% alcohol reflux, extracting solution reclaims ethanol and makes and contain amount of alcohol and be lower than 15%, placed 24 hours at cold place, separate out insoluble matter, centrifugal or filter, clear liquid with the petroleum ether extraction defat after, continue thin out to the extract color with n-butyl alcohol-ethyl acetate mixed extractant solvent of 4: 1, the enrichment flavone, concentrating under reduced pressure, remove the hybrid extraction solvent after, the concentrated solution thin up disperses, on the polyamide resin column handled well, first water is eluted to the Molish reaction and is negative, and continues the ethanol elution with 50%～80%, collect ethanol elution, concentrating under reduced pressure, drying is pulverized, get the Sticktight general flavone dry extract, wherein extract obtained general flavone content is more than or equal to 50%.
4. preparation method as claimed in claim 1, wherein said and the immiscible middle polarity organic solvent of water can be selected from any in mixing of ethyl acetate, n-butyl alcohol or both.
5. preparation method as claimed in claim 4, the mixed solvent of wherein said and the water preferred n-butyl alcohol of immiscible middle polarity organic solvent and ethyl acetate.
6. has application in blood pressure lowering, the blood lipid-lowering medicine by the Sticktight general flavone of gained in the described preparation method of each claim in the claim 1 to 5 in preparation.
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| CN102018741A (en) * | 2010-12-10 | 2011-04-20 | 安徽医科大学 | Spanishneedles herb total flavone extract as well as preparation technology and preparation thereof |
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| CN104825523A (en) * | 2015-04-20 | 2015-08-12 | 唐兴龙 | Wild chrysanthemum flower general flavone extraction method |
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| CN105748539A (en) * | 2016-02-26 | 2016-07-13 | 新疆维吾尔自治区药物研究所 | Juniperus sabina total flavonoid extract as well as preparation method and application thereof |
| CN105935371A (en) * | 2016-06-08 | 2016-09-14 | 常方圆 | Pharmaceutical application of total flavonoids of Bidens pilosa |
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| CN109939133A (en) * | 2019-04-28 | 2019-06-28 | 云南汉德生物技术有限公司 | A method of extracting general flavone from beggar-ticks |
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