CN102319275B - Sunset abelmoschus flower extract, preparation and preparation method thereof - Google Patents
Sunset abelmoschus flower extract, preparation and preparation method thereof Download PDFInfo
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- CN102319275B CN102319275B CN2011102833529A CN201110283352A CN102319275B CN 102319275 B CN102319275 B CN 102319275B CN 2011102833529 A CN2011102833529 A CN 2011102833529A CN 201110283352 A CN201110283352 A CN 201110283352A CN 102319275 B CN102319275 B CN 102319275B
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- Prior art keywords
- flos abelmoschi
- abelmoschi manihot
- extract
- manihot extract
- flos
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Landscapes
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a sunset abelmoschus flower extract, a preparation and a preparation method thereof. The sunset abelmoschus flower extract and the preparation have the advantages of high active ingredient content and stable quality; a preparation process is easy and convenient to operate, and is safe and reliable; a reasonable and practicable preparation method is provided for large-scale production of traditional Chinese medicines; and the problem of large dosage of a sunset abelmoschus flower preparation is solved.
Description
Technical field
Technology of the present invention belongs to field of traditional Chinese medicine pharmacy, is specifically related to a kind of Flos abelmoschi manihot extract, preparation and preparation method thereof.
Background technology
Flos abelmoschi manihot is the dried floral of Malvaceae Abelmoschus plant Abelmoschus manihot Abelmoschus Manihot (L.) Medic, and Flos abelmoschi manihot is recorded in " the good book on Chinese herbal medicine of helping " the earliest, and extensive, aboundresources distribute; Compendium of Material Medica record: its flower abnormal smells from the patient is sweet, cold, sliding, nontoxic, cures mainly urine leaching and expedites the emergence of, and controls at the malignant boil pus person that is not recovered for a long time; Do deposited promptly the healing in end; Be persons particularly liable to develop skin infection's key medicine, the cellulitis that disappears is swollen, and immersion oil is coated with burn etc.In the modern medicine, the main effective ingredient of Flos abelmoschi manihot is a flavones ingredient, at present to The Chemical Constituents also concentrate on Flos abelmoschi manihot total flavones (Total flavone of A, TFA) and monomer whose.From existing so far seven flavonoid monomer separation evaluation eighties in 20th century.The research proof has the reduction albuminuria, alleviates erythrocyturia, alleviates interstitial disease of renal tubule; Eliminate oxygen-derived free radicals, improve the erythrocyte immune adhesion, promote the transhipment and the removing of people's CIC ELISA (CIC); Regulate cellular immune function, suppress the humoral immune reaction degree, thereby alleviate people's CIC ELISA (CIC) mediation property injury of kidney; Improve renal function, reach the purpose of treatment chronic nephritis (CKD).The Radix seu folium abelmoschi moschati capsule that SZYY Group Pharmaceutical Limited. produces is a Flos abelmoschi manihot extract; Add the domestic exclusive listing product of processing behind the pharmaceutic adjuvant, be mainly used in the treatment chronic nephritis, clinical research shows; Total effective rate damp-heat syndrome group 78.95%, non-damp-heat syndrome group 62.12%; Treatment chyluria total effective rate 84.62%; The concurrent diabetic nephropathy of treatment non-insulin-dependent diabetes mellitus, the result shows the albuminuria that can significantly alleviate clinical phase diabetic nephropathy (DN), and in conjunction with blood sugar lowering, blood pressure lowering treatment, total effective rate is 83.87%, and remission rate is 25.81%, and is evident in efficacy.
Radix seu folium abelmoschi moschati is the extract of Malvaceae plant Flos abelmoschi manihot total flavones, and the method for preparing of total flavone extract of maniod eibish reduces three kinds at present:
1, first water or alcohol extraction are suspended from the extract mixture that reclaims solvent in the water, use chloroform, ethyl acetate, n-butanol extraction respectively, are divided into several extraction parts, reuse silicagel column or polydextran gel column chromatography, separate into the one pack system material.
2, use ethanol extraction, merge extractive liquid, filters; Filtrating concentrates, and concentrated solution adds the suitable quantity of water dilution, through macroporous resin column or pass through polyamide column; Use the alcohol-water solution gradient elution, eluent concentrates, drying; Get extractive of general flavone, the method for preparing of the total flavone extract of maniod eibish described in application number 200410035741.X patent of invention file after the pulverizing.
3, use ethanol extraction, proportion was the extractum of 1.13-1.16 when merge extractive liquid,, extracting solution were evaporated to 60 ℃, added boiling water gradation dissolving, left standstill, and filtered, and filtrating is used methanol-eluted fractions through macroporous adsorptive resins or polyamide column chromatography, collects eluent; Eluent concentrating under reduced pressure, vacuum drying get the total flavone extract of maniod eibish bullion; The extractive of general flavone crude product refining; With ethyl acetate-ethanol extraction; Reclaim solvent, drying under reduced pressure or vacuum drying obtain total flavone extract of maniod eibish, the method for preparing of the total flavone extract of maniod eibish described in application number 200610097615.6 patent of invention files.
Above-mentioned first method is the method for the single flavone component of laboratory research, is not suitable for the preparation of total flavones; Second method prepares the adsorption technology of using macroporous adsorptive resins or polyamide column in the process; Though macroporous resin or polyamide are a kind of effective process for purification refine active constituent-enriched, that remove impurity; But its porogen and catabolite are toxic; And cost was high during this technology was applied to produce greatly, the cycle is long, is not easy to big production industrialization flow process; The third method prepares the adsorption technology of having used macroporous adsorptive resins or polyamide column in the process equally; Be not suitable for big production industrialization flow process, in the drying under reduced pressure process, total flavone extract of maniod eibish lumps easily in addition; And the vacuum drying cycle is long; The coking phenomenon is serious, directly influences content, the quality of total flavone extract of maniod eibish, and the dosage that finally causes preparation once to be taken is big.
In view of the foregoing; Be badly in need of a kind of easy and simple to handle, safe and reliable, technology is rationally feasible, steady quality, Flos abelmoschi manihot total flavones method for preparing that extractive content is high; Be fit to the big production requirement of enterprise, more solved the big problem of Flos abelmoschi manihot preparation taking dose, make things convenient for the patient, benefit the patient.
Summary of the invention
The objective of the invention is to: a kind of more stable quality is provided, and technology is more convenient, effective ingredient is more complete, and preparation technology is simple, with low cost, the Flos abelmoschi manihot extract of suitable industrialized great production, preparation and preparation method thereof.Through Flos abelmoschi manihot total flavones method for preparing of the present invention; The content of total flavone extract of maniod eibish, low-quality problem have been solved; Method for preparing particularly of the present invention is fit to industrialized great production, easy and simple to handle, be easy to control, extract is dry rapidly, utilization method for preparing of the present invention during industrialization is produced; The content of Flos abelmoschi manihot extract is high, quality is high, has solved the big problem of Flos abelmoschi manihot taking dose.
For realizing the present invention, the present invention provides following technical scheme.
A kind of Flos abelmoschi manihot extract; According to listed as parts by weight: 1～20 part of Flos abelmoschi manihot; Total flavones contains Quercetin-3-robinoside, hyperin, isoquercitrin, Quercetin-3 '-glucoside, gossypitrin-3 '-glucoside, ampelopsin-3-glucoside, gossypitrin, ampelopsin, Quercetin flavone compound in the extract; It is characterized in that general flavone content is no less than 11.5mg/g in hyperin in the extract, comprise following method for preparing:
The Flos abelmoschi manihot alcohol reflux, backflow filters, and merging filtrate reclaims ethanol to the greatest extent, concentrates, and the oil reservoir on cold preservation liquid upper strata is removed in cold preservation, regulates pH value, and drying is removed the cold preservation liquid of upper strata oil reservoir, promptly gets Flos abelmoschi manihot extract.
Above-mentioned preferred manufacturing procedure is:
Flos abelmoschi manihot is with 85%～95% ethanol, reflux, extract, 2～3 times, each 1～2 hour; Filter, merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.20～1.35; Concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid, adjust pH 6.0～7.0; Thin layer rapid draing promptly gets Flos abelmoschi manihot extract.
The condition of above-mentioned thin layer rapid draing operation is: preheating thin layer rapid draing barrel surface temperature to 135 ℃～160 ℃; Air pressure is 0.3～0.6Mpa; Drum rotation speed is 2～4.5 minutes/commentaries on classics; Coated panel is plastic plate or corrosion resistant plate, and plastic plate is selected from polyethylene version, PVC plastic plate, PP plastic plate, PE plastic plate, polyfluortetraethylene plate, preferably polytetrafluoroethylene plate.
Above-mentioned barrel is available from the dry facility for granulating company limited of Changzhou ten thousand backbones; In order to be fit to big requirement of producing; Carried out scrap build, parameter setting apparatus and steam control valve have been installed by the starting drive place of barrel, and dismountable coated panel has been installed at the roller trough place.
Thin layer rapid draing barrel used in the present invention has advantage: 1. dry rate is fast, and medicinal liquid forms thin film on the barrel surface, and the heat and mass direction is consistent, promptly is dried in the process that barrel turns around; 2. easy control easy and simple to handle: be convenient to continuous production and realize the big production automation, but because power rapid adjustment and mertialess characteristics, be easy to timely control, be convenient to the adjustment of technological parameter and confirm; 3. drying time is short: the medicinal liquid that is dried on the cylinder outer wall, and be 2～4.5 minutes/commentaries on classics whole arid cycle, can improve work efficiency more than four times with the conventional drying compared with techniques; 4. good product quality: compare with the conventional drying method, like vacuum drying, because under the vacuum occasion, heat transmits very difficult through convection current, can only conduct and carry out, firing rate is slow, and energy consumption is big, and arid cycle is long, is prone to the coking phenomenon, influences product quality; Drying under reduced pressure, because the medicinal liquid inside and outside is not dry simultaneously, the about temperature difference of medicinal liquid is big, it is inhomogeneous about heating to occur, is prone to caking, influence product quality, and the present invention has overcome the defective of conventional drying method, rapid draing, product quality has raising by a relatively large margin.
Above-mentioned best method for preparing is:
Flos abelmoschi manihot is with 95% ethanol, and reflux, extract, 2 times each 1 hour, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.20, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 6.0 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till cold preservation liquid liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 140 ℃～150 ℃, air pressure is 0.4～0.5Mpa, opens the rollers roll start button; Drum speed is 3～3.5 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Above-mentioned Flos abelmoschi manihot extract; Can be mixed and made into various dosage forms with any or more than one adjuvant such as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, Pulvis Talci, calcium sulfate, micropowder silica gel, xylitol, lactose, glucose, glycine, mannitol, HP-s that meet medicinal standard etc.; Comprise oral formulations and ejection preparation, like tablet, slow releasing tablet, capsule, granule, soft capsule, drop pill, syrup, injection, infusion solution, injectable powder etc.Preferred dosage form is granule, tablet, capsule, injectable powder.
Above-mentioned Flos abelmoschi manihot extract is processed any preparation that medically allows, and contains Flos abelmoschi manihot total flavones and is no less than 5.7mg/g in hyperin.
Through Flos abelmoschi manihot total flavones method for preparing of the present invention; Resulting Flos abelmoschi manihot extract; According to listed as parts by weight: 1～20 part of Flos abelmoschi manihot; Extract general flavone content by weight percentage is 60.0%-95.0%, and the concrete component of wherein said total flavones is respectively: Quercetin-3-robinoside 3.0%-5.0%, hyperin 15.0%-24%, isoquercitrin 13.0%-19.0%, Quercetin-3 '-glucoside 9.0%-15.0%, gossypitrin-3 '-glucoside 7.0%-9.0%, ampelopsin-3-glucoside 2.5%-5.0%, gossypitrin 2.5%-5.0%, ampelopsin 2.5%-5.0%, Quercetin 5.5%-8.0%.
Through Flos abelmoschi manihot total flavones method for preparing of the present invention; Improved the content of Flos abelmoschi manihot total flavones effectively; Flos abelmoschi manihot total flavones by usual method is no less than 5.0mg/g in hyperin, brings up to Flos abelmoschi manihot total flavones and is no less than 5.7mg/g in hyperin.
Below come further to set forth the beneficial effect of Flos abelmoschi manihot extract of the present invention and preferred dosage form thereof through Test Example:
The present invention respectively organizes the experiment of Flos abelmoschi manihot extract treatment rat aminonucleoside nephropathy model
Experiment medicine: the Flos abelmoschi manihot extract of drying under reduced pressure (SZYY Group Pharmaceutical Limited.)
Vacuum drying Flos abelmoschi manihot extract (SZYY Group Pharmaceutical Limited.)
Flos abelmoschi manihot extract of the present invention (SZYY Group Pharmaceutical Limited.)
Laboratory animal: 40 of male SD rat, healthy adult (5 age in week), body weight 150 ± 25g/, Jiangsu Province's Experimental Animal Center provides.
Animal model: (puromycin aminoncleoside, PAN), U.S. sigma chemical company produces modeling medicine puromycin, modeling method, the disposable injection puromycin of rat abdominal cavity (PAN) 100mg/kg body weight.
Experimental technique: 40 of SD rats, adaptability was fed 7 days, was divided into 4 groups at random by body weight, 10 every group.
1) blank group: do not give any medicine, also not modeling.
2) the Flos abelmoschi manihot extract group of drying under reduced pressure: from beginning to irritate once a day the Radix seu folium abelmoschi moschati extract medicated powder 0.7g/kgd (being equivalent to raw medicinal herbs 8.4g/kgd) of clothes drying under reduced pressure, continuous two weeks modeling day.
3) vacuum drying Flos abelmoschi manihot extract: obey vacuum drying Radix seu folium abelmoschi moschati extract medicated powder 0.7g/kgd (being equivalent to raw medicinal herbs 8.4g/kgd), continuous two weeks from beginning modeling day to irritate once a day.
4) Flos abelmoschi manihot extract of the present invention: obey Radix seu folium abelmoschi moschati extract medicated powder 0.7g/kgd of the present invention (being equivalent to raw medicinal herbs 8.4g/kgd), continuous two weeks from beginning modeling day to irritate once a day.
All rats were all put to death in experiment on the 16th, and nephridial tissue is got in postmortem.Observe urine protein quantitation, kidney function test, blood fat analysis, plasma albumin, relevant free radical index situation, experimental result sees the following form.
Table 1 is respectively organized urine protein quantitation and is changed (mg/12hr mean SD)
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Table 2 is respectively organized the variation (mean SD) of blood biochemistry index first weekend
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Table 3 is respectively organized the variation (mean SD) of blood biochemistry index second weekend
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Table 4 is respectively organized blood SOD, MDA, P-O
- 2And R-O
- 2Level (mean SD)
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Table 5 is respectively organized body weight change (g mean SD)
Conclusion: show through above-mentioned test; The Flos abelmoschi manihot extract that makes through the present invention can significantly alleviate the urine albumen amount of aminonucleoside nephropathy model, alleviates edema, blood fat reducing; Improve kidney pathology; And tangible antioxidant radical is arranged, improve the effect of blood SOD vigor, and be certain dose-effect relationship.
The influence of xylol induced mice auricle edema
Laboratory animal: the Kunming kind is white mice 18-22g, and is male, male and female half and half, and China Academy of TCM's Experimental Animal Center provides.
Experiment medicine: the Flos abelmoschi manihot extract of drying under reduced pressure (SZYY Group Pharmaceutical Limited.)
Vacuum drying Flos abelmoschi manihot extract (SZYY Group Pharmaceutical Limited.)
Flos abelmoschi manihot extract of the present invention (SZYY Group Pharmaceutical Limited.)
Experimental technique: get 40 of white mice, be divided into 4 groups at random, 10 every group, i.e. blank group; Optional 3 groups, Radix seu folium abelmoschi moschati extract powder, vacuum drying Radix seu folium abelmoschi moschati extract, the Radix seu folium abelmoschi moschati extract of the present invention of difference gastric infusion drying under reduced pressure, every day 1 time, successive administration 4 days; After the last administration 1 hour, xylene 30 microlitres evenly are applied to the outside in the mouse right ear, the left side auricle is made own control; Cut auricle after 1 hour, take off auricle, weigh with the card punch of 9 millimeters of diameters; Calculate swelling rate and inhibitory rate of intumesce, the result compares the significance of difference between the administration group through the T check, and the result sees table 6.
Table 6 is respectively organized the influence of preparation xylol induced mice auricle edema
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Influence to granulation hyperplasia due to the agar
Laboratory animal: the Wister rat, male, body weight 150-200 gram, China Academy of TCM experimental animal center provides.
Experiment medicine: the Flos abelmoschi manihot extract of drying under reduced pressure (SZYY Group Pharmaceutical Limited.)
Vacuum drying Flos abelmoschi manihot extract (SZYY Group Pharmaceutical Limited.)
Flos abelmoschi manihot extract of the present invention (SZYY Group Pharmaceutical Limited.)
Experimental technique: 2 milliliters of subcutaneous 2% agar solutions with 56 ℃ of sterile working injections of rat back are divided into 4 groups after 24 hours, 10 every group at random; That is: the Flos abelmoschi manihot extract group (3g/kg) of blank group, drying under reduced pressure, vacuum drying Flos abelmoschi manihot extract group (3g/kg), Flos abelmoschi manihot extract group of the present invention (3g/kg) are pressed above-mentioned dosage gastric infusion respectively, every day 1 time; Continuously give 14 days, after the drug withdrawal second day, pentobarbital sodium anesthesia back was dissected and is separated agar granulation lump; Take by weighing weight in wet base; The swollen weight of each group represented with mean SD, checks the relatively significance of difference between the administration group through T, and the result sees table 7.
Table 7 is respectively organized preparation to granulomatous influence
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
To the experiment of water load rat diuresis
Laboratory animal: 40 of SD rat, body weight 150-280 gram, male and female half and half, experimental animal center, Jiangsu Province provides.
Experiment medicine: the Flos abelmoschi manihot extract of drying under reduced pressure (SZYY Group Pharmaceutical Limited.)
Vacuum drying Flos abelmoschi manihot extract (SZYY Group Pharmaceutical Limited.)
Flos abelmoschi manihot extract of the present invention (SZYY Group Pharmaceutical Limited.)
Experimental technique: the last late fasting of rat experiment, test and cut off the water in preceding 3 hours.After giving distilled water or administration, put into metabolic cage immediately.All squeeze out intravesical storage urine before and after the collection urine.Be divided into four groups at random, every group of 10 rats.The blank group, distilled water 3ml/100g body weight is irritated stomach.The Flos abelmoschi manihot extract of drying under reduced pressure, vacuum drying Flos abelmoschi manihot extract, Flos abelmoschi manihot extract of the present invention, are pressed the 3ml/100g body weight and are irritated stomach to 3ml with distilled water diluting, are equivalent to 0.6g crude drug/100g body weight.The feedwater of above-mentioned rat or administration morning every day once, for three days on end.Calculate each class mean and standard deviation, compare the significance of difference between the administration group through the T check, the result sees table 8, table 9.
Table 8 feed water first or administration after urine amount and urine electrolyte change (mean SD)
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Urine amount and urine electrolyte after table 9 feedwater in continuous three days or the administration change (mean SD)
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Influence to the rat platelet concentration
Laboratory animal: the Wister kind is a rat, and is male, body weight 157.3 ± 11.9g, and experimental animal center, Jiangsu Province provides.
Experiment medicine: the Flos abelmoschi manihot extract of drying under reduced pressure (SZYY Group Pharmaceutical Limited.)
Vacuum drying Flos abelmoschi manihot extract (SZYY Group Pharmaceutical Limited.)
Flos abelmoschi manihot extract of the present invention (SZYY Group Pharmaceutical Limited.)
Experimental technique: get 40 of rat, be divided into four groups at random, 10 every group, remove the blank group; Its excess-three group is pressed 6g/kg dosage gastric infusion or water respectively, every day 1 time, continuous 7 days; After the last administration 1 hour, use the pentobarbital sodium anesthetized animal, open abdomen and get blood 1.8ml; Transfer to immediately 3.8% sodium citrate 0.2ml is housed in vitro shake anti-hemostasis-coagulation gently, use the SchateShi improved method, measure platelet garden tree type (%) at Nippon Television video recording microscopically; Expansion type (%) and gather number, through the T check significance of difference between the administration group relatively, the result sees table 10.
Table 10 is respectively organized the influence of preparation to rat platelet aggregation property
Flos abelmoschi manihot extract group ratio with drying under reduced pressure
*P＜0.05 is with vacuum drying Flos abelmoschi manihot extract group ratio
*P＜0.01.
Conclusion: show that through pharmacological evaluation Flos abelmoschi manihot extract of the present invention has better pharmacological action.
The preparation that adopts method for preparing of the present invention to make, through 37-40 ℃, RH75 ± 5% is placed and was carried out stable accelerated test (seeing table 11) in 3 months.
Table 11 Flos abelmoschi manihot preparation stability result of the test
The result listed from last table shows that Flos abelmoschi manihot preparation of the present invention has good quality stability, and after 3 months, each item index does not have significant change in accelerated test condition held for it.
Medicine of the present invention is used for the situation of clinical observation:
1, physical data
Accept out-patient's totally 240 examples for medical treatment, male's 128 examples wherein, women's 112 examples.Age 18-30 year 28 examples, 31-40 year 32 examples, 41-50 year 44 examples, 51-70 year 16 examples.Wherein professional cadre 40 people, teacher 28 people, workman 32 people, driver 12 people, peasant 4 people, student 4 people.
2, diagnostic criteria
(1) tcm diagnosis standard
The chronic nephritis damp-heat syndrome
Primary symptom: 1) appearance or limbs edema.
2) waist distending pain, burning pain, percussion pain.
3) frequent pharyngalgia, the tonsillitis enlargement, or bring out the state of an illness because of last sense and increase the weight of.
4) skin furuncle and phyma, skin infection etc., or increase the weight of because of skin infection brings out the state of an illness.
5) urine is deep yellow, muddiness, and foam is many, hematuria, burning sensation during urination, puckery pain is unfavorable, or brings out the state of an illness because of urinary tract infection and increase the weight of.
6) yellowish fur, or the root of the tongue is yellow greasy, red tongue.
7) urine pus cell＞5/HP, or Urine sediments analyzer counting WBC＞400,000/hr.
Inferior disease: 1) bitter taste, halitosis, mouth is sticking, or xerostomia.
2) breast gastral cavity painful abdominal mass is vexed, and abdominal distention is indigestion and loss of appetite.
3) feel sick vomiting.
4) big loose stool dirt is unsmooth not well, or constipation with dry stool or close.
5) soft pulse art, or sliding art.
6) urine sialic acid (U
SA)＞90mg/L.
7) urine N-acet-beta-amino glucosidase (U
NAG)＞25
U/ L.
Allly possess primary symptom project 1), and time 1 the above person of disease that holds concurrently; Or 2 above persons of primary symptom; Or 3 above persons of inferior disease, can be diagnosed as this disease.
(2) Western medicine diagnose standard
Chronic nephritis
1) onset is slow, state of an illness delay, the time heavy when light, renal function can appear in the later stage progressively to go down, anemia, electrolyte disturbance, performances such as blood BUN, Cr rising.
2) in various degree performances such as albuminuria, hematuria, edema and hypertension are arranged, weight differs.
3) can bring out acute attack because of reasons such as respiratory tract infection in the course of disease, the performance of similar acute nephritis occur.
(3) chronic nephritis weight grade scale
The weight of the state of an illness is mainly judged from aspects such as albuminuria, renal function, edema, hypertension.All possess following any 1 and can confirm.
Slightly: 1) the urine protein qualitative examination continue +～++, or urine protein quantitation continues 1g/ below day, renal function is normal; 2) edema is not obvious, and blood pressure is normal.
Moderate: 1) the urine protein qualitative examination continues ++～+++, or lasting 1～2g/ day of urine protein quantitation, renal function is normal; 2) edema can gently can weigh, and hypertension can be arranged.
Severe: 1) the urine protein qualitative examination continues ++ +～++ ++, or lasting 2.1～3.5g/ day of urine protein quantitation (blood albumin＞30g/L); 2) renal dysfunction; 3) obvious edema and hypertension.
(4) Therapeutic Method
Flos abelmoschi manihot preparation of the present invention:
Oral Radix seu folium abelmoschi moschati capsule: one time 3, three times on the one.
Oral Radix seu folium abelmoschi moschati tablet: one time 3, three times on the one.
Oral Radix seu folium abelmoschi moschati granule: one time 1 bag, three times on the one.
Commercially available Radix seu folium abelmoschi moschati capsule: oral, one time 5, three times on the one.
8 weeks of continuous use.The part ratio of alleviating fully, alleviating basically continues 12 weeks of providing follow-up care for a patient.Complicated hypertension, glycosuria patient allow to continue to use the depressor of originally taking.
(5) efficacy assessment standard
1) curative effect classification
■ is alleviated fully: symptom such as edema and sign complete obiteration, urine protein examination continue negative or " ± ", or the twenty-four-hour urine protein quantification continues less than 0.2g, and urine erythrocyte disappears under the high power lens, and renal function is normal.
■ is alleviated basically: symptom such as edema and sign disappear basically, and the urine protein examination continuous decrease is more than 50%, and urine erythrocyte is no more than 3～5 under the high power lens, and renal function normally or normal basically (differ be no more than 15% with normal value).
■ takes a turn for the better: symptoms such as edema are clearly better with sign, one of urine protein examination continuous decrease+, or twenty-four-hour urine protein quantification continuous decrease 25～49%, urine erythrocyte is no more than 5～8 under the high power lens, and renal function is normally or improvement arranged.
■ is invalid: clinical manifestation and above-mentioned lab testing all do not have the obvious improvement or the person of increasing the weight of.
2) can not estimate: due to illness people's compliance or other masters, odjective cause can't accurately be estimated curative effect.
3) relatively reach the variation of treating front and back between each MAIN OUTCOME MEASURES group.
(6) efficacy analysis
Table 12 through a course of therapy after observation of curative effect
The result listed from last table shows, P＜0.05, and test group is superior to matched group, and Flos abelmoschi manihot preparation of the present invention has excellent curative.
Below the method for quality control of Flos abelmoschi manihot preparation of the present invention is studied:
(1) Flos abelmoschi manihot being carried out thin layer differentiates:
The thin layer discrimination method of Flos abelmoschi manihot: get the about 1g of these article, add ethyl acetate 50ml, heating and refluxing extraction 1 hour filters, and filtrating volatilizes, and residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets the Quercetin reference substance, adds ethanol and processes, and every 1ml contains the solution of 0.2mg, as reference substance solution.According to thin layer chromatography (appendix VI B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on the silica gel g thin-layer plate of same usefulness 0.5% sodium hydroxide solution preparation; With toluene-ethyl acetate-formic acid (5: 4: 1) is developing solvent; Launch, take out, dry; Spray is put under ultra-violet lamp (365) nm and is inspected with 1% aluminum trichloride solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(2) moisture: should cross 9.0% (appendix I XH second method).
(3) other: should meet regulation relevant under the corresponding preparations item.
(4) assay:
Chromatographic condition and system suitability test: use octadecyl silane to be filler; With mobile phase A: acetonitrile-0.1% phosphoric acid solution (15: 85), Mobile phase B: acetonitrile-0.1% phosphoric acid solution (25: 75), according to the form below carries out gradient elution; Flow velocity is per minute 1.0ml; The detection wavelength is 360nm; Column temperature is 30 ℃, and number of theoretical plate calculates by the hyperin peak should be not less than 35000.
The preparation of reference substance solution: the about 10mg of hyperin reference substance of 120 ℃ of vacuum drying to the constant weights of learning from else's experience, the accurate title, decide, and puts in the 100ml measuring bottle; Add the about 70ml of mobile phase A liquid, slight fever makes dissolving in water-bath, puts cold; Add mobile phase A and be diluted to scale, shake up, promptly get.
The preparation of need testing solution: get the content under these article content uniformity item, porphyrize is got 0.1g, and accurate the title decides, and puts in the 25ml measuring bottle; Add the about 15ml of methanol, supersound process 30 minutes is put coldly, adds methanol and is diluted to scale; Shake up, filter (0.45 μ m), get subsequent filtrate, promptly get with microporous filter membrane.
Algoscopy: accurate respectively reference substance solution and each 10～20 μ l of need testing solution of drawing, inject chromatograph of liquid, the record chromatogram, promptly gets with calculated by peak area by external standard method.
These article are pressed dry product and are calculated, and every contains Flos abelmoschi manihot with hyperin (C
21H
20O
12) calculate, must not be less than 5.7mg.
Below come further to set forth Flos abelmoschi manihot preparation of the present invention through embodiment method for preparing.
The specific embodiment
Flos abelmoschi manihot is the dried floral of Malvaceae (Malvaceae) Abelmoschus plant Abelmoschus manihot Abelmoschus Manihot (L.) Medic.
The Flos abelmoschi manihot raw material is provided by SZYY Group Pharmaceutical Limited. Abelmoschus manihot GAP planting base, and other raw materials are commercially available, and meets standards of pharmacopoeia.
Embodiment 1:
Raw medicinal material Flos abelmoschi manihot 2000g of the present invention
Flos abelmoschi manihot is with 95% ethanol, and reflux, extract, 2 times each 1 hour, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.20, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 6.0 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 140 ℃, air pressure is 0.4Mpa, opens the rollers roll start button; Drum speed is 3 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Said extracted thing general flavone content by weight percentage reaches 95.0%, and the concrete component of wherein said total flavones is respectively: Quercetin-3-robinoside 5.0%, hyperin 24.0%, isoquercitrin 19.0%, Quercetin-3 '-glucoside 15.0%, gossypitrin-3 '-glucoside 9.0%, ampelopsin-3-glucoside 5.0%, gossypitrin 5.0%, ampelopsin 5.0%, Quercetin 8.0%.
Embodiment 2:
Raw medicinal material Flos abelmoschi manihot 1000g of the present invention
Flos abelmoschi manihot is with 85% ethanol, and reflux, extract, 3 times each 2 hours, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.35, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 7.0 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 150 ℃, air pressure is 0.5Mpa, opens the rollers roll start button; Drum speed is 3.5 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Said extracted thing general flavone content by weight percentage reaches 80.0%, and the concrete component of wherein said total flavones is respectively: Quercetin-3-robinoside 4.5%, hyperin 19.0%, isoquercitrin 18.0%, Quercetin-3 '-glucoside 14.0%, gossypitrin-3 '-glucoside 8.0%, ampelopsin-3-glucoside 3.5%, gossypitrin 3.5%, ampelopsin 3.5%, Quercetin 6.0%.
Embodiment 3:
Raw medicinal material Flos abelmoschi manihot 800g of the present invention
Flos abelmoschi manihot is with 90% ethanol, and reflux, extract, 2 times each 2 hours, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.30, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 6.5 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 150 ℃, air pressure is 0.5Mpa, opens the rollers roll start button; Drum speed is 3.5 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Said extracted thing general flavone content by weight percentage reaches 85.0%, and the concrete component of wherein said total flavones is respectively: Quercetin-3-robinoside 4.5%, hyperin 20.0%, isoquercitrin 17.0%, Quercetin-3 '-glucoside 14.0%, gossypitrin-3 '-glucoside 8.5%, ampelopsin-3-glucoside 4.5%, gossypitrin 4.5%, ampelopsin 4.5%, Quercetin 7.5%.
Embodiment 4:
Raw medicinal material Flos abelmoschi manihot 100g of the present invention
Flos abelmoschi manihot is with 95% ethanol, and reflux, extract, 3 times each 2 hours, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.20, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 6.0 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 145 ℃, air pressure is 0.4Mpa, opens the rollers roll start button; Drum speed is 3 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Said extracted thing general flavone content by weight percentage reaches 60.0%, and the concrete component of wherein said total flavones is respectively: Quercetin-3-robinoside 3.0%, hyperin 15.0%, isoquercitrin 13.0%, Quercetin-3 '-glucoside 9.0%, gossypitrin-3 '-glucoside 7.0%, ampelopsin-3-glucoside 2.5%, gossypitrin 2.5%, ampelopsin 2.5%, Quercetin 5.5%.
Embodiment 5:
Raw medicinal material Flos abelmoschi manihot 1500g of the present invention
Flos abelmoschi manihot is with 95% ethanol, and reflux, extract, 2 times each 1 hour, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.20, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 6.0 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 160 ℃, air pressure is 0.6Mpa, opens the rollers roll start button; Drum speed is 2 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Said extracted thing general flavone content by weight percentage reaches 75.0%, and the concrete component of wherein said total flavones is respectively: Quercetin-3-robinoside 4.0%, hyperin 22.0%, isoquercitrin 15.0%, Quercetin-3 '-glucoside 13.0%, gossypitrin-3 '-glucoside 8.0%, ampelopsin-3-glucoside 3.0%, gossypitrin 3.0%, ampelopsin 3.0%, Quercetin 4.0%.
Embodiment 6:
Raw medicinal material Flos abelmoschi manihot 900g of the present invention
Flos abelmoschi manihot is with 90% ethanol, and reflux, extract, 3 times each 2 hours, is filtered; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.30, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃, removed the oil reservoir of cold preservation liquid; Adjust pH 6.5 slowly adds cold preservation liquid in the thin layer rapid draing roller trough, till liquid level and barrel surface being rigidly connected touch; Preheating barrel surface temperature to 135 ℃, air pressure is 0.3Mpa, opens the rollers roll start button; Drum speed is 4.5 minutes/commentaries on classics, the extractum liquid that tumbles is coated on the polyfluortetraethylene plate lowers the temperature, and waits to dry the material cooling and becomes fragile; Break into pieces, pack in the clean double-layer plastic bag, promptly get Flos abelmoschi manihot extract.
Embodiment 7:
Flos abelmoschi manihot extract (embodiment 1 method makes) 400g
After the Flos abelmoschi manihot extract pulverizing, add hydroxypropyl cellulose, Pulvis Talci, microcrystalline Cellulose, the calcium sulfate mixing of above-mentioned weight portion, cross 80 mesh sieves; Add an amount of dehydrated alcohol, system soft material, reuse 20 mesh sieve system granules; Drying, granulate, encapsulated; Process 1000 altogether, every contains Flos abelmoschi manihot total flavones and counts 7.2mg/g with hyperin.
Embodiment 8:
Flos abelmoschi manihot extract (embodiment 2 methods make) 400g
After the Flos abelmoschi manihot extract pulverizing, add microcrystalline Cellulose, the Icing Sugar mix homogeneously of above-mentioned weight portion, add 3% polyvidone alcoholic solution and make soft material in right amount; Cross 18 mesh sieves, 60 ℃ of dryings 30～45 minutes, granulate; Add Pulvis Talci, mixing, granulate; Pack is processed 1000 bags altogether, contains Flos abelmoschi manihot total flavones and counts 6.8mg/g with hyperin.
Embodiment 9:
Flos abelmoschi manihot extract (embodiment 4 methods make) 400g
After Flos abelmoschi manihot extract, low-substituted hydroxypropyl methylcellulose, magnesium stearate pulverize separately crossed 80 mesh sieves, mix homogeneously added ethanol solution and makes soft material in right amount, crossed 20 mesh sieves; 60 ℃ of dryings 30～45 minutes, granulate adds microcrystalline Cellulose; Mixing, tabletting is pressed 1000 altogether.Contain Flos abelmoschi manihot total flavones and count 6.7mg/g with hyperin.
Embodiment 10:
Flos abelmoschi manihot extract (embodiment 3 methods make) 400g
Flos abelmoschi manihot extract is mixed with process heat sterilization, clarifying edible vegetable oil and Cera Flava fused mass, fully stir and promptly get capsule core material.Get gelatin and add suitable quantity of water and make its expansion, glycerol and proper amount of water for injection are put be heated to 70 ℃～80 ℃ in the glue pot, mix homogeneously; Add expansible gelatin and stir, fusing, insulation; Left standstill 1-2 hour, and removed the foam on upper strata, take advantage of heat filtering; Place the gelatin groove, 60 ℃ of temperature slowly add Flos abelmoschi manihot extract in the gelatin groove; The liquid paraffin temperature is advisable with 25 ℃, 15 ℃～20 ℃ of room temperatures, 50 ℃～60 ℃ of water dropper temperature, beginning drop pill.The soft gelatin capsule that oozes evenly spreads out on the gauze conveyer belt, and soft gelatin capsule surface paraffin is removed in 10 ℃ of low temperature blowing 6 hours, 10 ℃ of low temperature blowings 24 hours, and 45 ℃ of dryings 12 hours are removed useless ball, after the assay was approved, packing.Contain Flos abelmoschi manihot total flavones and count 7.0mg/g with hyperin.
Embodiment 11:
Flos abelmoschi manihot extract (embodiment 5 methods make) 400g
HP-225g
Mannitol 115g
Water for injection is an amount of
After the Flos abelmoschi manihot extract pulverizing, HP-225g stirring and evenly mixing, the water for injection of 5 times of amounts of adding stirs; 60 ℃ were stirred 1～2 hour, added mannitol 115g, stirred and made dissolving, adjust pH 7.0; Add the injection water to cumulative volume, continue to stir after 10 minutes, ultrafiltration, the filtrating fill is in cillin bottle; Lyophilization, is added a cover at tamponade, promptly gets.Contain Flos abelmoschi manihot total flavones and count 6.9mg/g with hyperin.
Embodiment 12:
Flos abelmoschi manihot extract (embodiment 6 methods make) 400g
After the Flos abelmoschi manihot extract pulverizing, add hydroxypropyl cellulose, Pulvis Talci, microcrystalline Cellulose, the calcium sulfate mixing of above-mentioned weight portion, cross 80 mesh sieves; Add an amount of dehydrated alcohol, system soft material, reuse 20 mesh sieve system granules; Drying, granulate, encapsulated; Process 1000 altogether, every contains Flos abelmoschi manihot total flavones and counts 6.6mg/g with hyperin.
Claims (10)
1. Flos abelmoschi manihot extract, it is characterized in that: total flavones contains Quercetin-3-robinoside, hyperin, isoquercitrin, Quercetin-3 '-glucoside, gossypitrin-3 '-glucoside, ampelopsin-3-glucoside, gossypitrin, ampelopsin, Quercetin in the extract, and general flavone content is no less than 11.5mg/g in hyperin in the extract; The method for preparing of said Flos abelmoschi manihot extract is following: Flos abelmoschi manihot is with 85%～95% ethanol, reflux, extract, 2～3 times, each 1～2 hour; Filter; Merging filtrate reclaims ethanol to most, concentrated filtrate to proportion 1.20～1.35, and concentrated solution left standstill 24～48 hours at 0 ℃～4 ℃; Remove the oil reservoir of cold preservation liquid; Adjust pH 6.0～7.0, thin layer rapid draing promptly gets Flos abelmoschi manihot extract;
The condition of said thin layer rapid draing operation is: preheating thin layer rapid draing barrel surface temperature to 140 ℃～150 ℃, air pressure is 0.4～0.5MPa, drum speed be 3～3.5 minutes/change, coated panel is plastic plate or corrosion resistant plate.
2. Flos abelmoschi manihot extract according to claim 1 is when is characterized in that thin layer rapid draing, till cold preservation liquid liquid level and barrel surface rigidly connect and touch in the roller trough.
3. Flos abelmoschi manihot extract according to claim 1, when it is characterized in that thin layer rapid draing, wherein coated panel is polyethylene board, PVC plastic plate, PP plastic plate, PE plastic plate, polyfluortetraethylene plate.
4. Flos abelmoschi manihot extract according to claim 1, when it is characterized in that thin layer rapid draing, wherein coated panel is a polyfluortetraethylene plate.
5. Flos abelmoschi manihot extract according to claim 1 is characterized in that with the Flos abelmoschi manihot extract being medicinal raw material, processes granule behind the adding pharmaceutic adjuvant.
6. Flos abelmoschi manihot extract according to claim 1 is characterized in that with the Flos abelmoschi manihot extract being medicinal raw material, processes capsule behind the adding pharmaceutic adjuvant.
7. Flos abelmoschi manihot extract according to claim 1 is characterized in that with the Flos abelmoschi manihot extract being medicinal raw material, processes soft capsule behind the adding pharmaceutic adjuvant.
8. Flos abelmoschi manihot extract according to claim 1 is characterized in that with the Flos abelmoschi manihot extract being medicinal raw material, processes tablet behind the adding pharmaceutic adjuvant.
9. Flos abelmoschi manihot extract according to claim 1 is characterized in that with the Flos abelmoschi manihot extract being medicinal raw material, processes injectable powder behind the adding pharmaceutic adjuvant.
10. according to any described Flos abelmoschi manihot extract of claim 5～9, it is characterized in that containing in the preparation Flos abelmoschi manihot total flavones and be no less than 5.7mg/g in hyperin.
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| CN102600219B (en) | 2012-03-21 | 2013-02-13 | 江苏苏中药业集团股份有限公司 | Total flavone extract of abelmoschus manihot and preparing method of total flavone extract |
| CN103977015B (en) * | 2014-05-05 | 2016-10-05 | 南京瑞菁医药科技有限责任公司 | Chinese medicine saussurea intybus Lipid-lowering activities components compatibility compositions |
| CN103976466B (en) * | 2014-05-20 | 2016-06-01 | 河南中烟工业有限责任公司 | The application of yellow hollyhock seed extract in cigarette |
| CN104082852B (en) * | 2014-07-24 | 2015-12-09 | 中国烟草总公司郑州烟草研究院 | The application of sunset abelmoschus root extract in cigarette shreds |
| CN106120139B (en) * | 2016-07-15 | 2019-03-08 | 浙江真爱时尚家居有限公司 | A kind of production technology of tencel fiber woollen blanket |
| CN107519220A (en) * | 2017-09-15 | 2017-12-29 | 江苏苏中药业集团股份有限公司 | The extracting method of flavone compound in a kind of sunset abelmoschus flower |
| CN110075138A (en) * | 2019-05-17 | 2019-08-02 | 江苏苏中药业集团股份有限公司 | A kind of granule of maniod ebish flower extract and preparation method thereof |
| CN110051851A (en) * | 2019-05-31 | 2019-07-26 | 江苏苏中药业集团股份有限公司 | A kind of combination of sodium-glucose co-transporter -2 inhibitor and maniod ebish flower extract |
| CN111920836B (en) * | 2019-06-13 | 2023-04-18 | 苏中药业集团股份有限公司 | Application of abelmoschus manihot extract in preparation of medicine for treating fibrosis |
| WO2023173268A1 (en) * | 2022-03-15 | 2023-09-21 | 苏中药业集团股份有限公司 | Effective parts of flavonoids from flos abelmoschus manihot, and preparation method therefor and use thereof |
| CN116270775B (en) * | 2023-04-19 | 2023-10-27 | 杭州康恩贝制药有限公司 | Abelmoschus manihot total flavone effective part extract and industrialized mass production preparation process thereof |
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| CN102319275A (en) | 2012-01-18 |
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