CN101474275A - Preparation method and application of Chinese medicine extract for 'prescription for treating diarrhoea with abdominal pain' - Google Patents
Preparation method and application of Chinese medicine extract for 'prescription for treating diarrhoea with abdominal pain' Download PDFInfo
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Abstract
The invention discloses a preparation method for a Chinese herbal extract 'prescription for treating diarrhoea with abdominal pain', comprising the following steps: (1) fried rhizoma atractylodis macrocephalae, white paeony root, fried dried orange peel and divaricate saposhnikovia root are taken as raw materials, alcohol solution or water is taken as solvent to extract the raw materials to obtain the extracting solution; the weight ratio of the raw materials is as follows: fried rhizoma atractylodis macrocephalae: white paeony root: fried dried orange peel: divaricate saposhnikovia root is equal to 1:1:0.75:0.5; (2) the obtained extracting solution is concentrated until the volume of the extracting solution is 6-9 times of the weight of the raw materials, namely, 1kg of the raw materials corresponds to 6-9L of extracting solution; (3) the concentrated solution obtained in step (2) is diluted by water with 3-5 times of volume and then the supernatant is extracted; (4) the supernatant is absorbed by macroporous resin column, the eluted part of the alcohol is collected to obtain the alcohol eluent; (5) the obtained alcohol eluent is concentrated and dried to prepare the Chinese herbal extract. The invention also relates to the application of the Chinese herbal extract 'prescription for treating diarrhoea with abdominal pain' prepared by the method in preparing the medicines for curing irritable bowel syndrome of intestinal canal.
Description
Technical field
The present invention relates to a kind of preparation method of Chinese medicine extract, relate in particular to the preparation method of the Chinese medicine extract that is used for the treatment of the intestinal irritable bowel syndrome.
The invention still further relates to according to the Chinese medicine extract of above-mentioned preparation method preparation with and application in preparation treatment intestinal irritable bowel syndrome medicine.
Background technology
Intestinal irritable bowel syndrome (Irritable bowelsyndrome, IBS) be modal clinically a kind of function of intestinal canal disorder disease, mainly showing as stomachache, abdominal distention, constipation, diarrhoea or constipation and diarrhoea and replace, is one of modal digestive system disease.The IBS prevalence is about 5.7% among the crowd of China community, western countries IBS crowd prevalence is more than 10%, sickness rate very high various places, whole world sickness rate between 10%～15%, main cause spiritedness factor, infective agent, alteration of intestinal flora, inherited genetic factors etc.At present, the concrete typing of IBS has three kinds on spastic colon type (based on lower abdomen especially lower-left stomachache and constipation), painless property diarrhea-type (serves as to lead with mucus with diarrhoea), mixed type, so the curative of this indication has significant values.
At present, Therapeutic Method on Western medicine, mainly contain employing diarrhea such as loperamide, diphenoxylate, spasmolytic such as atropine, probanthine, papaverine, trimebutine, dynamics-promoting medicine such as cisapride, 5-HT etc., but these medicines all have more side effect and untoward reaction, modal untoward reaction is constipation and acute ischemia colitis as cisapride, serious side effects to cardiovascular system, the atropine untoward reaction is more, as aroused in interestly overrun, blurred vision, agitation, hallucination, xerostomia etc., show particularly evidently the old people, clinical use should be prudent.And Chinese medicine has advantage to the wholistic therapy of this disease, is still most important Therapeutic Method.Classical Chinese medicine tradition prescription tongxieyao formula is the representative of such disease of treatment.
Irritable bowel syndrome does not have this name of disease in motherland's medical science, and primary disease belongs to " intestinal is strongly fragrant " category in " traditional Chinese medical science disease method of treatment term ", sporadically appears in the document of classes such as Chinese medicine " stomachache ", " diarrhoea ", " constipation "." tcm clinical practice diagnosis and treatment term disease part " regulation: intestinal is strongly fragrant to be " because of feelings will is not relaxed, the mechanism of qi retardance makes the intestinal dysfunction of the spleen in transportation and transformation, is the strongly fragrant sick class disease of common performance with stomachache, diarrhoea or constipation ".The card that pain is rushed down is by deficient earth being subjugated by wood, and incoordination between the liver and spleen is due to board fortune is not normal." hospital examines " said: " rush down the spleen of duty, the liver of severely rebuking; The liver duty is real, the void of spleen duty, and insufficiency of the spleen excess of the liver is so the order pain is rushed down." be characterized in rushing down and must suffer from abdominal pain.Control suitable spleen reinforcing subduing the hyperfunction of the liver, eliminating dampness to stop diarrhea." tongxieyao formula " history is stated from Jing-Yue Complete Works, mainly consists of four flavor Chinese medicines such as the Rhizoma Atractylodis Macrocephalae, the Radix Paeoniae Alba, Pericarpium Citri Reticulatae, Radix Saposhnikoviae in the side, and the Rhizoma Atractylodis Macrocephalae is bitter sweet and warm in the side, and spleen reinforcing dampness is empty to control soil, is monarch drug.Radix Paeoniae Alba acid is cold, and the easing the affected liver relieving spasm to stop pain matches with the Rhizoma Atractylodis Macrocephalae, and Yu Tuzhong rushes down wood, is ministerial drug.Pericarpium Citri Reticulatae is arduous and warm, the dampness of regulating the flow of vital energy, and the board stomach function regulating of waking up is adjuvant drug.The property that a small amount of Radix Saposhnikoviae of compatibility, tool rise to loose, with art, Chinese herbaceous peony mutually 5, the hot stagnation of liver-QI of loosing, the perfume temper of relaxing, and dampness is arranged to help the merit of antidiarrheal, and be again the medicine of board through tying-in, make it usefulness so have concurrently to help.Four medicines are harmonious, and can spleen reinforcing win wet and antidiarrheal, and easing the affected liver is regulated the flow of vital energy and pain relieving, makes the strong liver of spleen gentle, and pain is rushed down from ending.
" tongxieyao formula " is as a prescription of well treating irritable bowel syndrome, but its applicating and exploitation does not have the market finished product to promote, only be limited at present the decoction use of clinician to prescription, reason is a just decoction of its extract preparation, it is further used be restricted.
The preparation technology of " tongxieyao formula " extract, put down in writing by the successive dynasties prescription, all be " Rhizoma Atractylodis Macrocephalae is fried two liang of [6g] Radix Paeoniae Alba and is fried two liang [6g], and Pericarpium Citri Reticulatae is fried one or two 5 money [4.5g]; Radix Saposhnikoviae one or two [3g]; on fritter, divide and make eight clothes, decocting or ball clothes ", the tradition prescription is an extract for the decocting thing, this extract is not easy keeping because be decocting liquid, and is perishable, mobile big, viscosity is strong, if further be processed into related preparations, the moisture absorption of product is very strong, mildew easily, its contained main active is not high, and volume is big, and the dosage form that processing and preparing is new is very difficult.Therefore, the preparation technology of the extract of this prescription is necessary to further investigate, makes its extract still can meet or exceed the curative effect of former water extract, and technology is simple, and is feasible, is fit to suitability for industrialized production, be convenient to further develop various preparations, be convenient to market and extensively promote.
Summary of the invention
The technical study of " tongxieyao formula " Chinese medicine extract is attempted ining all sorts of ways, as solvent method, the soda acid method, macroporous resin method is furtherd investigate, determined a kind of preparation technology of novel macroporous resin method at last, implement preparation method, finished its industrialized preparation technology preferably.
Therefore, one object of the present invention is to provide a kind of preparation method (following tongxieyao formula Chinese medicine extract that also claims of Chinese medicine extract, or tongxieyao formula extract), it is a foundation with Chinese Chinese medicine prescription " tongxieyao formula ", and the new preparation method of this prescription Chinese medicine is provided.
Another object of the present invention is to provide a kind of Chinese medicine extract with the inventive method preparation.
A further object of the present invention is to provide the application of Chinese medicine extract of the present invention in preparation treatment intestinal irritable bowel syndrome medicine.
According to an aspect of the present invention, Chinese medicine extract of the present invention is a feedstock production with the Chinese medicine medical material Rhizoma Atractylodis Macrocephalae, the Radix Paeoniae Alba, Pericarpium Citri Reticulatae and Radix Saposhnikoviae.Wherein the Rhizoma Atractylodis Macrocephalae is that the feverfew Rhizoma Atractylodis Macrocephalae (Atractylodes macrocephalaKoidz) rhizome, the Radix Paeoniae Alba are that dry root, the Pericarpium Citri Reticulatae of ranunculaceae plant Radix Paeoniae (Paeonia lactiflora Pall.) is the dry mature skin of rutaceae orange (Citrus reticulata Blanco) and variety thereof, and Radix Saposhnikoviae is the dry root of umbelliferae Saposhnikovia divaricata (Saposhnikovia divaricata (Turcz.) Schischk.).Can adopt the medical material that crude drug is concocted again as required in the preparation, for example Rhizoma Atractylodis Macrocephalae (parched), Radix Paeoniae Alba (parched), stir-fry Pericarpium Citri Reticulatae etc.The Chinese medicine extract that obtains is the mixture of the collaborative onset of contained various activity of drug ingredients composition, and it is different from activated monomer, its drug effect also be different from simply adding of various activity of drug ingredients composition drug effects and.
According to an aspect of the present invention, provide a kind of preparation method of tongxieyao formula Chinese medicine extract, comprise the steps:
1) being raw material with Rhizoma Atractylodis Macrocephalae (parched), Radix Paeoniae Alba (parched), stir-fry Pericarpium Citri Reticulatae and Radix Saposhnikoviae, is the described raw material of solvent extraction with alcoholic solution or water, obtains extracting solution; Each raw material weight is than being Rhizoma Atractylodis Macrocephalae (parched): Radix Paeoniae Alba (parched): fry Pericarpium Citri Reticulatae: Radix Saposhnikoviae=1:1:0.75:0.5;
2) extracting solution that concentrate to obtain to the volume of described extracting solution is 6～9 times of described raw material weight, is equivalent to 1Kg raw material correspondence 6～9L extracting solution;
3) with 3～5 times of volume water dilution step 2) concentrated solution that obtains, get supernatant;
4) described supernatant is adsorbed with macroporous resin column, collect the ethanol elution part, obtain ethanol elution;
5) concentrate the also dry ethanol elution that obtains, obtain described Chinese medicine extract.
Wherein, in the step 1), described alcoholic solution or extraction with aqueous solution are meant with aquiferous ethanol or water as solvent, for example adopt routine techniques known in the art, extractions such as heat reflow method, percolation, continuous countercurrent technique, the solvent for use volume is about 10 times of medical material weight, i.e. the corresponding 10L solvent of 1Kg medical material.For instance, can adopt volumetric usage is that 60～75% ethanol water of 8～10 times of medical material weight carries out hot reflux and extracts; Extraction time is 2～3 times; Heating-up temperature can be 70～85 ℃.
Step 2) in, after extracting solution concentrated, its volume was preferably 6～9 times of crude drug weight.
In the step 3), concentrated solution is preferably to add the water dilution of 3～5 times of volumes.
In the step 4), behind the adsorption column adsorbing and extracting liquid, preferably use the water washing of 1～5BV (bed volume), eluent flow rate is preferably 0.5～2.5BV/hr; Eluting ethanol preferably adopts 50～70% ethanol waters, and eluent flow rate is preferably 0.5～2.5BV/hr.
The bed volume behind the resin that loads for resin column of BV (Bed Volum) wherein.The disposal ability of resin column is directly proportional with its resin useful load.The flow of eluent and speed are unit of account with BV or BV/hr.
Described macroporous resin is generally the middle polarity adsorbent resin that contains ester group or cyano group of styrene type copolymer, and its structure is the macroporous netlike structure, for example D-101 macroporous resin, SIPI-40 macroporous resin, SIPI-21 macroporous resin or SIPI-8 macroporous resin etc.
Before last sample, earlier macroporous resin is carried out pre-treatment, run off from waste liquid to prevent effective ingredient.When the resin pre-treatment, use earlier the 5%HCl eluting, the back is washed till neutrality with purified water, reuse 2%NaOH eluting, the back is washed till neutrality with purified water, during continuous production, washes post with 95% ethanol, and the back is washed till with purified water and does not contain ethanol, can reuse.
In the step 5), the extract that obtains carries out dried, obtains the extract of dried forms, and used drying means comprises vacuum drying, spray drying and lyophilization etc.
Therefore, further, the preparation method of Chinese medicine extract of the present invention may further comprise the steps:
A). with Rhizoma Atractylodis Macrocephalae (parched), Radix Paeoniae Alba (parched), stir-fry Pericarpium Citri Reticulatae and Radix Saposhnikoviae is raw material, and the alcoholic solution hot reflux with 60～75% is extracted 2～3 times, merge extractive liquid;
B). it is 6～9 times of raw-material weight that extracting solution is evaporated to volume;
C). with the water dilution concentrated solution of 3～5 times of volumes, and clarification, get supernatant;
D). described supernatant is adsorbed the abandoned stream fluid with macroporous resin column; With the water of 1～5BV, wash described adsorption column with 0.5～2.5BV/ hour flow velocity, abandon water lotion; Afterwards, adopt 50～70% ethanol,, collect this ethanol elution with 0.5～2.5BV/ hour flow velocity eluting adsorption column;
E). concentrated, dry ethanol elution obtain described Chinese medicine extract.
In addition, before adopting above-mentioned prepared extract, can earlier this medical material be carried out pre-treatment, be about to the medical material cleaning, drying, pulverize, sieve.
The present invention further adopts high performance liquid chromatography that the extract of above-mentioned prepared is carried out content control, and has set up with the rapid analysis method under a kind of chromatographic condition.
According to a further aspect in the invention, according to " tongxieyao formula " Chinese medicine extract of the inventive method preparation, it contains 4～7% Hesperidin by weight, 2～4% peoniflorin, 0.1～0.4% cimicifugoside and 0.5～1.5% atractylodes lactone.
The content control of mentioned component, adopt the content of high performance liquid chromatography (HPLC) mensuration by Hesperidin, peoniflorin, cimicifugoside, atractylodes lactone in the Chinese medicine extract for preparing, with Hesperidin, peoniflorin, cimicifugoside, atractylodes lactone is reference substance, and mensuration obtains.
Chinese medicine extract provided by the invention can be treated irritable bowel syndrome, syndrome of stagnation of liver qi and spleen deficiency, syndrome of spleen-deficiency, damp-heat stagnating in the spleen, acute enteritis, chronic colitis, nervous diarrhea etc.Therefore, the invention still further relates to the application of this Chinese medicine extract in the above-mentioned disease medicament of preparation treatment, relate in particular to the application in the medicine for preparing the treatment irritable bowel syndrome.
The acute toxicity tests shows, this Chinese medicine extract is through the gastric infusion approach, the appetite of ICR mice, body weight no abnormality seen, LD50〉10.0g/kg, show that toxicity is low, have good drug safety.
Chinese medicine extract of the present invention can also further be formed pharmaceutical composition with pharmaceutically acceptable carrier and/or excipient etc.For example, a kind of pharmaceutical composition can be that extractive of general flavone and pharmaceutically acceptable carrier and/or excipient mix according to certain proportioning; Can also be that extractive of general flavone, other Chinese medicine extract and pharmaceutically acceptable carrier and/or excipient are mixed according to certain proportioning.
Aforementioned pharmaceutical compositions can further be mixed with the form that can supply with medicine according to the conventional formulation method, comprises per os or parenteral form.In the form that can supply with medicine, should comprise the extract for the treatment of effective dose.It is so-called that " the treatment effective dose " is meant that under this dosage the extract of the present invention symptom of can improving or palliate a disease maybe can suppress or block advancing of disease.
The compositions that can supply with medicine can be tablet, capsule, powder, granule, lozenge, suppository, patch, gel, powder or liquid preparation (as oral or aseptic parenteral solution or suspension).These compositionss that can supply with medicine can also be prepared into sustained-release preparation or targeting preparation as required.
The form of oral administration can be tablet, capsule, powder, granule etc., and they can contain conventional excipients such as binding agent as syrup, arabic gum, gelatin, sorbitol, Tragacanth, hydroxypropyl emthylcellulose or polyvinylpyrrolidone; Filler such as lactose, sucrose, corn starch, calcium phosphate, sorbitol or glycine; Tabletting lubricant such as magnesium stearate; Disintegrating agent such as starch, polyvinylpyrrolidone, crospovidone, sodium starch glycolate or microcrystalline Cellulose or pharmaceutically acceptable wetting agent such as sodium lauryl sulphate.
Fluid composition (as liquid oral compositions) can be prepared as emulsion, syrup or elixir form, perhaps they is prepared as the desciccate form, water or other suitable solvent dissolving before use.This type of liquid preparation can contain conventional additive, as suspending agent as sorbitol, syrup, methylcellulose, gelatin, hydroxyethyl-cellulose, carboxymethyl cellulose, aluminium stearate gel, hydrogenation edible fat; Emulsifying agent such as lecithin, Arlacel-80 or arabic gum; Water-insoluble solvent (can comprise edible oil) is as almond oil, fractionated coconut oil, oily ester such as glycerol, propylene glycol or alcoholic acid ester; Antiseptic such as methyl parahydroxybenzoate or propyl ester or sorbitol; And can contain conventional correctives or coloring agent if desired.
Reactive compound and aseptic solvent as described in parenteral compositions (as the parenteral compositions) can contain, according to the concentration of using, described reactive compound can be suspended in or be dissolved in this solvent.When preparing the solution of parenteral, compositions of the present invention can be dissolved in the water for injection filtration sterilization, fill also sealing in suitable glass tube vial or ampoule then.As described in preferably adjuvant being dissolved in as local anesthetic, antiseptic and buffer agent in the solvent.For increasing stability, freezing after the said composition fill is in glass tube vial and vacuum can be removed moisture.Can prepare the parenteral suspension with essentially identical method, but described reactive compound is to be suspended in the solvent rather than to be dissolved in the solvent, and degerming can not be undertaken by filtration.Described chemical compound can be sterilized by being exposed in the oxirane, then it is suspended in the aseptic solvent.Preferably contain surfactant or wetting agent in the said composition to help the uniform distribution of active component.
The present invention possesses following advantage:
1, preparation technology's enrichment main active effectively of extract provided by the invention such as Hesperidin, peoniflorin, cimicifugoside, atractylodes lactone etc. make the prescription of its content far above direct water extract; Quality control adopts high efficient liquid phase analysis method to carry out assay, and is simple and easy to control.
2, adopt the resin purification method among the extract preparation technology provided by the invention, this method is easy, quick, favorable reproducibility; Selected absorption with macroporous adsorbent resin amount is big, and desorption efficiency is big, can use repeatedly, reduces the technology cost; Selected etoh solvent, inexpensive, nontoxic.
3, the extract that obtains of preparation technology of the present invention is compared with the decocting thing of former prescription, and volume is little, Chinese medicine inherent quality height, and the product moisture absorption reduces, stability increases, and anti-to control the effect of intestinal irritable bowel syndrome more obvious; And make the various dosage forms of appearance looks elegant easily.
4, The acute toxicity tests shows, the toxicity of extractive of general flavone is low, has good drug safety, and this has fully pointed out the clinical application safety of the extract of this prepared.
Therefore, " tongxieyao formula " Chinese medicine extract described in the present invention is fit to suitability for industrialized production, has very strong practicality.
The specific embodiment
By the following examples essence that the present invention may be better understood, but do not limit the present invention in any way.
Material source: the Rhizoma Atractylodis Macrocephalae is that the feverfew Rhizoma Atractylodis Macrocephalae (Atractylodes macrocephala Koidz) rhizome, the Radix Paeoniae Alba are that dry root, the Pericarpium Citri Reticulatae of ranunculaceae plant Radix Paeoniae (Paeonia lactiflora Pall.) is the dry mature skin of rutaceae orange (Citrus reticulata Blanco) and variety thereof, and Radix Saposhnikoviae is the dry root of umbelliferae Saposhnikovia divaricata (Saposhnikovia divaricata (Turcz.) Schischk.).Rhizoma Atractylodis Macrocephalae (parched), Radix Paeoniae Alba (parched) and stir-fry Pericarpium Citri Reticulatae are the Chinese crude drug of concocting again on the basis of the above-mentioned medical material Rhizoma Atractylodis Macrocephalae, the Radix Paeoniae Alba and Pericarpium Citri Reticulatae, and commercial the purchase obtains.Other materials is all bought by commercial sources.
One preparation " tongxieyao formula extract " of [embodiment 1] macroporous resin method
Get 50 kilograms of Chinese crude drug Rhizoma Atractylodis Macrocephalae (parched)s, 50 kilograms of Radix Paeoniae Alba (parched)s, fry 38 kilograms of Pericarpium Citri Reticulataes, 25 kilograms of Radix Saposhnikoviaes add 1 ton 75% ethanol, and heating and refluxing extraction 2h filters, and medicinal residues continue to add 1 ton of 75% alcohol reflux 2h, filter the merging of extracted twice liquid.Decompression and solvent recovery, 80 ℃ of temperature are concentrated to 9 times of volumes of crude drug, concentrated solution is added 5 times of hot water dilutions, add an amount of Chinese medicine clarifier chitosan, centrifugal, go precipitation, get supernatant, be splined on the D101 macroporous resin column and (before last sample, use acid, alkali respectively, water, alcohol carries out pre-treatment to resin column), wash described adsorption column with 5BV water (regulating PH with 1% hydrochloric acid is 5～6) earlier behind the last sample, abandon water lotion; The neutral 5BV aqueous solution of reuse eluting, the aqueous solution reject is used 70% ethanol elution of 5BV instead, and eluent flow rate is 2.5BV/h, collects this ethanol elution.Continue decompression and solvent recovery, collect extractum, spray drying, promptly.
Two preparations " tongxieyao formula extract " of [embodiment 2] macroporous resin method
Get 50 kilograms of Chinese crude drug Rhizoma Atractylodis Macrocephalae (parched)s, 50 kilograms of Radix Paeoniae Alba (parched)s, fry 38 kilograms of Pericarpium Citri Reticulataes, 25 kilograms of Radix Saposhnikoviaes add 1 ton of water, and heating and refluxing extraction 3h filters, and medicinal residues continue to add 1 ton of water reflux, extract, 2h, filter, and extracted twice liquid merges.Decompression and solvent recovery, 80 ℃ of temperature are concentrated to 6 times of volumes of crude drug, concentrated solution is added 3 times of hot water dilutions, add an amount of Chinese medicine clarifier chitosan, centrifugal, go precipitation, get supernatant, be splined on the D101 macroporous resin column and (before last sample, use acid respectively, alkali, water, alcohol carries out pre-treatment to resin column), earlier use the 2BV pure water rinsing behind the last sample, the aqueous solution reject is used 50% ethanol elution of 3BV instead, eluent flow rate is 2.0BV/h, collects this ethanol elution.Continue decompression and solvent recovery, collect extractum, spray drying, promptly.
The determination of bioactive constituent of [embodiment 3] tongxieyao formula extract
1. chromatographic condition
High performance liquid chromatograph HP1100 series (hewlette-packard), strong to close silica gel be filler with octadecylsilane, C18 chromatographic column, specification are 5 μ m, 4 * 250mm, 30 ℃ of column temperatures, water (A) and acetonitrile (B) they are mobile phase, gradient elution, UV-detector (UV) detects wavelength 230nm.
2. the preparation of " pain cathartic side " Chinese medicine extraction matter sample
1) extract of the present invention
Make each 3 lot number of above-mentioned Chinese medicine extract respectively by the embodiment of the invention 1 and 2 described methods.
2) direct water extract (former side's process)
Get 50 kilograms of Chinese crude drug Rhizoma Atractylodis Macrocephalae (parched)s, 50 kilograms of Radix Paeoniae Alba (parched)s, fry 38 kilograms of Pericarpium Citri Reticulataes, 25 kilograms of Radix Saposhnikoviaes add 1 ton of water, and heating and refluxing extraction 3h filters, and medicinal residues continue to add 1 ton of water reflux, extract, 2h, filter, and extracted twice liquid merges.Get the extracting solution that 1000ml merges, concentrate, drying obtains " pain cathartic side " Chinese medicine water extract.According to said method, make 3 lot numbers of direct water extract.
3) direct ethanol extract
Get 50 kilograms of Chinese crude drug Rhizoma Atractylodis Macrocephalae (parched)s, 50 kilograms of Radix Paeoniae Alba (parched)s, fry 38 kilograms of Pericarpium Citri Reticulataes, 25 kilograms of Radix Saposhnikoviaes add 1 ton 75% ethanol, and heating and refluxing extraction 2h filters, and medicinal residues continue to add 1 ton of 75% alcohol reflux 2h, filter the merging of extracted twice liquid.Get the extracting solution that 1000ml merges, concentrate, drying obtains " pain cathartic side " Chinese medicine ethanol extract.According to said method, make 3 lot numbers of direct ethanol extract.
3. the preparation of standard solution
Get that reference substance contains Hesperidin hesperidin, peoniflorin Paeoniflorin, cimicifugoside eimicifugoside, atractylodes lactone atractylode I are respectively 20.61mg, 15.34mg, an amount of dissolve with methanol of 14.22mg, 17.45mg, mix standardize solution in the volumetric flask of 100ml, shake up, make storing solution.Accurate draw an amount of storing solution, with methanol constant volume to the volumetric flask of 50ml.With reference substance concentration (x) is abscissa, and trap (y) is carried out regression Calculation for vertical coordinate, gets the regression curve of standard substance separately.
4. assay method
The above-mentioned Chinese medicine extraction matter sample of getting each lot number respectively is an amount of, accurate claim to conclude a contract or treaty be transferred to 25mg in the 50ml volumetric flask, add methanol 40ml, ultrasonic 30min under the room temperature takes out cool to room temperature, adds methanol to scale, shakes up, draw in right amount, be settled to 50ml, shake up, can measure.Can calculate each component content according to standard curve.The results are shown in Table 1:
Each constituent content measurement result of table 1.
| Hesperidin (%) | Peoniflorin (%) | Cimicifugoside (%) | Atractylodes lactone (%) | |
| Embodiment 1,2 is totally 6 lot numbers | 4～7 | 2～4 | 0.1～0.4 | 0.5～1.5 |
| Direct 3 lot numbers of water extract | 2～4 | 1～2 | 0.05～0.09 | 0.3～0.45 |
| Direct 3 lot numbers of ethanol extract | 3～5 | 1～2 | 0.07～0.09 | 0.3～0.45 |
From result of study as can be known, in the above-mentioned Chinese medicine extract by the inventive method preparation, contain Hesperidin hesperidin, peoniflorin Paeoniflorin, cimicifugoside eimicifugoside, atractylodes lactone atractylodeI are respectively 4～7%, 2～4%, 0.1～0.4%, 0.5～1.5%.Each constituent content all is higher than direct water extract and ethanol extract.
[embodiment 4] " tongxieyao formula " Chinese medicine extract is to the effect of mice intestinal propulsion functions
Get 140 of healthy Kunming kind white mice, body weight 18～225g, male and female half and half, be divided into 7 groups at random, every group 20, i.e. blank group, positive controls (bismuth subcarbonate), the basic, normal, high dosage group of tongxieyao formula extract of the embodiment of the invention 1 preparation, totally 7 groups of the direct water extract of tongxieyao formula, the direct ethanol extract of tongxieyao formula.Press table 2 dosage to mice continuous irrigation stomach (ig) administration 12d, fasting 24h before determination experiment.Be mixed with 8% charcoal end suspension with 10% arabic gum, 1h intravenous injection charcoal end suspension 20mlkg after the last administration, 20min puts to death animal afterwards, dissect, measure charcoal end head end displacement and small intestinal total length (from pylorus to ileocecus) in intestinal tube, calculate each group of tongxieyao formula extract the charcoal end is advanced percentage rate.
Experimental result shows, with the blank group relatively, each group of tongxieyao formula extract advances percentage rate all obviously to reduce to the charcoal end, shows that they all can reduce the enteral carbon powder and advance length, at the body intestinal motility obvious suppression effect being arranged.Simultaneously, be that the effect of the high, medium and low dosage of tongxieyao formula extract is stronger to the bowel movement inhibitory action by the sample of embodiment 1 preparation, illustrate than the direct water of former prescription and carry or the more remarkable treatment effect of the product of alcohol extraction.The results are shown in Table 2:
Table 2. tongxieyao formula extract is to the influence of mice intestinal function
| Group | Number of animals | Dosage (g/Kg) | Advance percentage rate (%) |
| The blank group | 20 | 0 | 80.12±4.67 |
| Tongxieyao formula extract low dose group | 20 | 1 | 55.23±6.15＊ |
| Dosage group in the tongxieyao formula extract | 20 | 2 | 50.34±6.11★ |
| Tongxieyao formula extract high dose group | 20 | 3 | 48.64±3.44★ |
| The direct water extract of tongxieyao formula | 20 | 3 | 60.22±2.13＊ |
| The direct ethanol extract of tongxieyao formula | 20 | 3 | 61.37±6.68＊ |
| Bismuth subcarbonate | 20 | 0.14 | 63.12±5.23* |
Compare * P＜0.01, ★ P＜0.005 with matched group.
Claims (7)
1. the preparation method of " tongxieyao formula " Chinese medicine extract may further comprise the steps:
1) being raw material with Rhizoma Atractylodis Macrocephalae (parched), Radix Paeoniae Alba (parched), stir-fry Pericarpium Citri Reticulatae and Radix Saposhnikoviae, is the described raw material of solvent extraction with alcoholic solution or water, obtains extracting solution; Each raw material weight is than being Rhizoma Atractylodis Macrocephalae (parched): Radix Paeoniae Alba (parched): fry Pericarpium Citri Reticulatae: Radix Saposhnikoviae=1:1:0.75:0.5;
2) extracting solution that concentrate to obtain to the volume of described extracting solution is 6～9 times of described raw material weight, is equivalent to 1Kg raw material correspondence 6～9L extracting solution;
3) with 3～5 times of volume water dilution step 2) concentrated solution that obtains, get supernatant;
4) described supernatant is adsorbed with macroporous resin column, collect the ethanol elution part, obtain ethanol elution;
5) concentrate the also dry ethanol elution that obtains, obtain described Chinese medicine extract.
2, the described preparation method of claim 1 is characterized in that comprising the steps:
A) described raw material is with 60～75% alcoholic solution heating and refluxing extraction 2～3 times, merge extractive liquid;
B) concentrating under reduced pressure gained extracting solution to the volume of described extracting solution is 6～9 times of raw-material weight, obtains concentrated solution;
C) with the water dilution concentrated solution of 3～5 times of volumes, supernatant is got in clarification;
D) described supernatant is crossed macroporous resin column absorption, abandoned stream fluid; Use the water of 1～5BV then, wash described adsorption column, abandon water lotion with 0.5～2.5BV/ hour flow velocity; Afterwards, adopt 50～70% ethanol, elution volume 3～5BV with 0.5～2.5BV/ hour flow velocity eluting adsorption column, collects ethanol elution;
E) concentrated, dry described ethanol elution obtains " tongxieyao formula " Chinese medicine extract.
3, the described preparation method of claim 2, the adsorbing material that it is characterized in that described macroporous resin column are D-101 macroporous resin, DIPI-40 macroporous resin, DIPI-21 macroporous resin or SIPI-8 macroporous resin.
4, a kind of " tongxieyao formula " Chinese medicine extract with the described preparation method preparation of claim 1.
5, claim 4 described " tongxieyao formula " Chinese medicine extract is characterized in that containing in the described extract Hesperidin 4～7%, peoniflorin 2～4%, cimicifugoside 0.1～0.4% and atractylodes lactone 0.5～1.5% by weight.
6, a kind of pharmaceutical composition is characterized in that containing claim 4 described " tongxieyao formula " Chinese medicine extract, and further comprises pharmaceutically acceptable carrier and/or excipient.
7, claim 4 described " tongxieyao formula " Chinese medicine extract is in the application of preparation treatment intestinal irritable bowel syndrome.
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| CN103735685A (en) * | 2013-12-30 | 2014-04-23 | 南京欣通瑞亿医药科技有限公司 | Chinese herb extract composition for treating functional gastrointestinal disorder or irritable bowel syndrome, preparation method and application of composition to preparation of medicine |
| CN104189170A (en) * | 2014-08-20 | 2014-12-10 | 王彩云 | Traditional Chinese medicine capsule for treating spleen deficiency and liver stagnation symptom and preparation method thereof |
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| CN103735685A (en) * | 2013-12-30 | 2014-04-23 | 南京欣通瑞亿医药科技有限公司 | Chinese herb extract composition for treating functional gastrointestinal disorder or irritable bowel syndrome, preparation method and application of composition to preparation of medicine |
| CN104189170A (en) * | 2014-08-20 | 2014-12-10 | 王彩云 | Traditional Chinese medicine capsule for treating spleen deficiency and liver stagnation symptom and preparation method thereof |
| CN104435254A (en) * | 2014-11-18 | 2015-03-25 | 中国中医科学院西苑医院 | Traditional Chinese medicine for treating myelodysplastic syndrome and prepration method of traditional Chinese medicine |
| WO2018154064A1 (en) * | 2017-02-24 | 2018-08-30 | Bioactor Bv | Flavanones for use in treating visceral hypersensitivity |
| US11141420B2 (en) | 2017-02-24 | 2021-10-12 | Bioactor Bv | Flavanones for use in treating visceral hypersensitivity |
| CN107213449A (en) * | 2017-07-04 | 2017-09-29 | 金云龙 | A kind of Chinese medicine preparation for being used to treat diarrhea before dawn |
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