CN103356801B - Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology - Google Patents
Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology Download PDFInfo
- Publication number
- CN103356801B CN103356801B CN201310313541.5A CN201310313541A CN103356801B CN 103356801 B CN103356801 B CN 103356801B CN 201310313541 A CN201310313541 A CN 201310313541A CN 103356801 B CN103356801 B CN 103356801B
- Authority
- CN
- China
- Prior art keywords
- weight portion
- bazhen
- keli
- radix
- parched
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention provides a method for preparing bazhen granules by low-temperature continuous extraction combined with membrane separation technology, including the steps of: preparing traditional Chinese medicine decoction pieces of eight herbs including codonopsis pilosula and rhizoma atractylodis macrocephalae; mixing angelica sinensis, ligusticum wallichii and stir-bake rhizoma atractylodis macrocephalae, continuously extracting by ethanol at low temperature, recovering ethanol, decocting the dregs of angelica sinensis, ligusticum wallichii and stir-bake rhizoma atractylodis macrocephalae after continuous extraction at low temperature with water, decocting codonopsis pilosula, poria cocos, prepared rehmannia root and honey-fried licorice root with water, mixing the extracts, using an ultrafiltration membrane with a molecular weight cutoff of 8000-12000 for separation and purification, concentrating the liquid filtered by the membrane, standing, concentrating supernatant to an extract, adding accessories to the extract, and making into sugar-containing granules and sugar-free granules. The method is high in extraction efficiency, low in energy consumption, automatic in continuous operation; can remove the non-medicinal ingredients, at the same time keep medicinal ingredients well, is substantially reduced in extracted extract, solves the difficult problem of forming bazhen granules, and is stable in product quality and low in cost.
Description
Technical field:
The present invention relates to the preparation of BAZHEN KELI, specifically a kind of low temperature (50 ~ 70 DEG C) extracts the method that binding film isolation technics prepares BAZHEN KELI continuously.
Background technology:
BAZHEN KELI is made up of Radix Codonopsis, Rhizoma Atractylodis Macrocephalae (parched), Poria, Radix Glycyrrhizae Preparata, Radix Angelicae Sinensis, Radix Paeoniae Alba (parched), Rhizoma Chuanxiong, Radix Rehmanniae Preparata eight taste Chinese medicine.BAZHEN KELI has invigorating qi and benefiting blood function, is used for the treatment of QI and blood deficiency, shallow complexion, inappetence, limbs fatigue, menorrhagia.
At present, the preparation method of BAZHEN KELI has some documents and patent report, Chinese patent application: 98112016.4 preparation methoies disclosing a kind of Bazhen sugar-free granule.Which disclose a kind of preparation method of Sugarless type BAZHEN KELI, the method is first by the Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis and Rhizoma Chuanxiong alcohol reflux, use soak by water again, obtain intermediate products, then Radix Codonopsis, Poria, Radix Rehmanniae Preparata, Radix Glycyrrhizae and the Radix Paeoniae Alba is added, and with soak by water, after filtration, concentrated after add excipient, granulate, after drying product Sugarless type BAZHEN KELI.The method uses alcohol heating reflux to extract, its reflux, extract, temperature higher (generally at 80 ~ 100 DEG C), and the heat-sensitive ingredients easily in destruction BAZHEN KELI as ferulic acid, thus makes the active constituent content of extraction reduce; In addition, owing to employing heating and refluxing extraction method, therefore increase the energy consumption of production, add production cost.In addition, the extraction of the method alcohol heating reflux and water boiling and extraction add the method that excipient makes BAZHEN KELI after filtering rear, direct concentrating, the extractum amount of the BAZHEN KELI extract be prepared from is larger, adjuvant proportion is less, easily occur being difficult to preparations shaping, the easy moisture absorption caking problem such as cause Moisture high UCL, character defective, makes product quality defective, affect the suitability for industrialized production of medicine, be difficult to the demand meeting doctor and patient.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, there is provided one effectively to retain active ingredient, removing, without active ingredient, is extracted extractum amount and is significantly reduced, BAZHEN KELI molding is easy, and more stable, that cost the is low low temperature of product quality extracts the method that binding film isolation technics prepares BAZHEN KELI continuously.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of low temperature extracts the method that binding film isolation technics prepares BAZHEN KELI continuously, and preparation process comprises:
(1) BAZHEN KELI crude drug formula: Radix Codonopsis 50-70 weight portion, Rhizoma Atractylodis Macrocephalae (parched) 50-70 weight portion, Poria 50-70 weight portion, Radix Glycyrrhizae Preparata 20-40 weight portion, Radix Angelicae Sinensis 80-100 weight portion, Radix Paeoniae Alba (parched) 50-70 weight portion, Rhizoma Chuanxiong 40-50 weight portion, Radix Rehmanniae Preparata 80-100 weight portion;
(2) according to step (1) BAZHEN KELI crude drug formula, first take Radix Angelicae Sinensis wherein, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) mixing, open steam solvent preheater and start heating extraction solvent; Open solvent pump, heating after Extraction solvent---the ethanol injection of 70%-80% is in rotocel extractor, and Extraction solvent temperature controls at 60 ~ 65 DEG C, and solvent injection rate is 1950-2050L/h; Then open feeding system, put in rotocel extractor continuously by above-mentioned Radix Angelicae Sinensis, Rhizoma Chuanxiong, the mixed medical material of Rhizoma Atractylodis Macrocephalae (parched), it is 180-220kg/h that medical material drops into speed, and opens solvent circulating pump; Start to receive after the 1.5 ~ 2.0h that feeds intake and extract solution, extract solution and after filter, go to transfer storage tank by feed pump, enter enrichment process; After the 2.0h that feeds intake, open desolventizing machine concentrate extraction solution precipitation, the preliminary heating zone temperature of desolventizing machine controls at 80 ~ 90 DEG C, and zone of heating temperature controls at 90 ~ 100 DEG C, and baking zone temperature controls, at 90 ~ 100 DEG C, to obtain medicinal residues, and ethanol reclaims;
(3) the 3-4 times amount that added water by the medicinal residues that the Radix Angelicae Sinensis of step (2) gained, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) are formed decocts 1.5-2 hour, filters and obtains the first filtrate, for subsequent use; All the other Radix Codonopsis, Poria, the Radix Paeoniae Alba, Radix Rehmanniae Preparata, Radix Glycyrrhizae Preparata 5 taste decoct with water 2 times according to after formula mixing, each 1-1.5 hour, amount of water is 5-6 times of above-mentioned 5 taste Chinese medicines for the first time, second time amount of water is the 3-4 times amount of above-mentioned 5 taste Chinese medicines, filter after decocting, the filtrate and the second filtrate that merge twice decoction are for subsequent use;
(4) combining step (3) two kinds of filtrates, select molecular weight cut off (molecular cut off) be 8000 ~ 12000 ultrafilter membrane carry out separation and purification, get ultrafiltration membrane permeate liquid, put in single-effect external circulation concentrator or the dense device of economic benefits and social benefits concentrated, during solution to be concentrated 85 DEG C, relative density (relative to water) stops concentrated to 1.10-1.15, clarify more than 24 hours, get supernatant; To be transferred to by above-mentioned supernatant in vacuum concentrator concentrated, when making 50 DEG C-60 DEG C, relative density (relative to water) is the extractum of 1.35 ~ 1.38;
(5) in the extractum of step (4) gained, add excipient and/or correctives, through granulation, dry, granulate, make granule and obtain BAZHEN KELI product.
The BAZHEN KELI product that the present invention is above-mentioned, to make 1000 weight portion sugar-containing type BAZHEN KELI (containing sucrose, being made up of extractum+sucrose+other excipient) meter, wherein extractum: (sucrose+other excipient sums) weight ratio=1:4 ~ 6; To make 300 weight portion Sugarless type BAZHEN KELI (without sucrose, be made up of other excipient+correctivess of extractum+except sucrose) meter, wherein extractum: weight ratio=1:1.5 ~ 3 of excipient, correctives wherein accounts for 0.3 ~ 0.9 weight portion of Sugarless type BAZHEN KELI.
Excipient described in step of the present invention (5) is at least one or two kinds and above mixture in sucrose, dextrin, soluble starch, starch, pregelatinized Starch.
Correctives described in step of the present invention (5) is aspartame, stevioside, acesulfame potassium (acesulfame potassium) at least one or two kinds and above mixture.
In step of the present invention (1) formula, each raw material is according to " Chinese Pharmacopoeia " and " Zhejiang Province's Chinese medicine processing specification " standard and the prepared slices of Chinese crude drugs raw material requiring to carry out concocting, making.
The invention has the advantages that:
1. the present invention adopts low temperature to extract binding film isolation technics continuously to prepare BAZHEN KELI.Adopt low temperature sequential extraction method, ensure that the heat-sensitive ingredients such as the ferulic acid in BAZHEN KELI effectively retain, reduce energy consumption, automaticity is high, overcomes that heating and refluxing extraction efficiency is low, energy consumption is high, can not the shortcoming of automatization's continued operation; Adopt membrane separation technique, select molecular weight cut off be 8000 ~ 12000 ultrafilter membrane, molecular weight is greater than 8000 ~ 12000 macromole invalid components to remove, and the active ingredient effectively retained within molecular weight 8000 ~ 12000, both active ingredient can be retained, solve again BAZHEN KELI and extract the excessive problem of extractum amount, solve BAZHEN KELI preparations shaping more difficult, a difficult problem for quality instability.
2. in the BAZHEN KELI that prepared by the present invention, alnulin acetas molecular weight 468.75, alnulin molecular weight 426.72, suberone molecular weight 426.72; Active ingredient in the Rhizoma Atractylodis Macrocephalae, atractylol molecular weight 182.22, atractylone 216.32, butenolide A 230.30; Active ingredient in Poria, pachymic acid molecular weight 528.76, eburicoic acid molecular weight 470.73, pachyman molecular weight 414.72; Chinese medicine of licorice root effect composition, glycyrrhizin (glycyrrhizic acid) molecular weight 822.92, liquirtin molecular weight 418.39, isoliquiritin molecular weight 418.39; Active ingredient in Radix Angelicae Sinensis, ligustilide molecular weight 190.24; Active ingredient in the Radix Paeoniae Alba, peoniflorin molecular weight 480.45, Hydroxy peoniflorin molecular weight 496.46, lactone glucoside of Radix Paeoniae molecular weight 480.46, benzoylpaeoniflorin molecular weight 584.57; Active ingredient in Rhizoma Chuanxiong, ligustrazine molecular weight 136.2, ferulic acid molecular weight 194.18; Active ingredient in Radix Rehmanniae, catalpol molecular weight 362.33, aucubin molecular weight 346.33.Visible, in BAZHEN KELI, active ingredient mostly is the composition of molecular weight, thus select molecular weight cut off be 8000 ~ 12000 ultrafilter membrane, successfully remain above-mentioned active ingredient.
Accompanying drawing explanation
Fig. 1 the inventive method prepares the process chart of extractum.
Flat turn extract technology flow chart in Fig. 2 the inventive method.
Detailed description of the invention
Below by embodiment, the present invention is described in further detail, but the present invention is not only confined to following examples.
Embodiment 1
Get Radix Codonopsis, Radix Angelicae Sinensis, Rhizoma Chuanxiong, Radix Rehmanniae, the Rhizoma Atractylodis Macrocephalae, Radix Glycyrrhizae, the Radix Paeoniae Alba, Poria medical material, arrange by Chinese Pharmacopoeia version in 2010 and " Zhejiang Province's Chinese medicine processing specification " (version in 2005), concoct, make each prepared slices of Chinese crude drugs.
Radix Codonopsis decoction pieces: get codonopsis pilosula, removing impurity, cleans, runs through, cut sheet, dry.
Angelica sinensis: get Radix Angelicae Sinensis medical material, removing impurity, cleans, runs through, shave, dry or cold drying.
Ligusticum wallichii decoction piece: get Ligusticum chuanxiong Hort, removing impurity, separately size, slightly bubble, clean, run through, shave, dry.
Radix Rehmanniae Preparata decoction pieces: get Radix Rehmanniae medical material, removing impurity, clean, moistening, cuts sheet, dry, and according to the steaming of steaming method to black profit, when taking-up is shone dry to about eighty per cant, cut sheet or block, drying, to obtain final product.
Rhizoma Atractylodis Macrocephalae (parched) decoction pieces: get Rhizoma Atractylodis Macrocephalae, removing impurity, clean, run through, cut sheet, drying then processed with honey wheat bran is sprinkled in hot pot, in time smoldering, adds Rhizoma Atractylodis Macrocephalae sheet, fries to coke yellow, and effusion burnt odor gas, take out, sieve removes processed with honey wheat bran.
Radix Glycyrrhizae Preparata decoction pieces: extracting liquorice medical material, removing impurity, cleans, runs through, cut sheet, dry.Take out when frying tack-free to buff to yellow according to processed with honey method, dry in the air cool.
Radix Paeoniae Alba (parched) decoction pieces: get white Peony Root, cleans, runs through, shave, dry.Fry to micro-yellow according to frying method.
Poria decoction pieces: get Poria, soaks, and cleans, slightly steams, cut skin and block in time or cut sheet, drying after profit.
Embodiment 2
Take the prepared slices of Chinese crude drugs after concocting in embodiment 1 respectively, Radix Codonopsis 48K weight portion, Rhizoma Atractylodis Macrocephalae (parched) 48K weight portion, Poria 48K weight portion, Radix Glycyrrhizae Preparata 24K weight portion, Radix Angelicae Sinensis 72K weight portion, Radix Paeoniae Alba (parched) 48K weight portion, Rhizoma Chuanxiong 36K weight portion, Radix Rehmanniae Preparata 72K weight portion, for subsequent use.
The Radix Angelicae Sinensis taken, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) are mixed, first open steam solvent preheater and start heating, open solvent pump, 75% ethanol is carried out extracting (Extraction solvent temperature controls between 60 ~ 65 DEG C) with the solvent injection rate of 2000L/h, until solvent makes rotocel extractor to last lattice visor; Open feeding system again, drop into medical material continuously with the speed of 200kg/h, and open solvent circulating pump one by one; Start to receive after the 1.5h that feeds intake and extract solution, feed liquid goes to transfer storage tank by pump after filter, enters enrichment process; After the 2.0h that feeds intake, open desolventizing machine, open steam valve and control the preliminary heating zone temperature of desolventizing machine at 80 ~ 90 DEG C, zone of heating temperature is at 90 ~ 100 DEG C, and baking zone temperature is at 90 ~ 100 DEG C, and medicinal residues reclaim ethanol through desolventizing machine.
4 times amount that Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) filtering residue added water decoct 2 hours, and decocting liquid filters, for subsequent use.All the other Radix Codonopsis, Poria, the Radix Paeoniae Alba, Radix Rehmanniae Preparata, Radix Glycyrrhizae Preparata 5 taste decoct with water 2 times (Poria is decocted a drug wrapped), each 1.5 hours, and amount of water is respectively 6 times, 4 times amount, and filter, merging filtrate is for subsequent use.
Merge above-mentioned filtrate, select molecular weight cut off be 10000 ultrafilter membrane carry out separation and purification, get ultrafiltration membrane permeate liquid, put single-effect external circulation concentrator or the dense device of economic benefits and social benefits to concentrate, solution to be concentrated relative density, to 1.10-1.15 (85 DEG C), is clarified more than 24 hours, is got supernatant.Medicinal residues adopt horizontal centrifugal, get filtrate, for subsequent use.Above-mentioned supernatant is transferred to vacuum concentrator concentrate, makes the extractum that relative density is 1.35 ~ 1.38 (50 DEG C-60 DEG C heat are surveyed).
Above-mentioned extractum is divided into quarter, for subsequent use.
Embodiment 3
Preparation in the Example 2 and extractum that obtain is a, adding excipient is sucrose and appropriate dextrin, through granulating, drying, granulate, make granule 200K weight portion, be packaged into 8 weight portions/bag, obtain sugar-containing type BAZHEN KELI product.
Embodiment 4
Preparation in the Example 2 and extractum that obtain is a, adds appropriate soluble starch and appropriate acesulfame potassium, through granulating, drying, granulate, make granule 60K weight portion, be packaged into 3.5 weight portions/bag, obtain Sugarless type BAZHEN KELI product.
Embodiment 5
Preparation in the Example 2 and extractum that obtain is a, adding excipient is sucrose and appropriate amount of starch, through granulating, drying, granulate, make granule 200K weight portion, be packaged into 8 weight portions/bag, obtain sugar-containing type BAZHEN KELI product.
Embodiment 6
Preparation in the Example 2 and extractum that obtain is a, adds appropriate pregelatinized Starch and appropriate acesulfame potassium, through granulating, drying, granulate, make granule 60K weight portion, be packaged into 3.5 weight portions/bag, obtain Sugarless type BAZHEN KELI product.
Embodiment 7
Take the prepared slices of Chinese crude drugs after concocting in embodiment 1 respectively, Radix Codonopsis 24K weight portion, Rhizoma Atractylodis Macrocephalae (parched) 24K weight portion, Poria 24K weight portion, Radix Glycyrrhizae Preparata 12K weight portion, Radix Angelicae Sinensis 36K weight portion, Radix Paeoniae Alba (parched) 24K weight portion, Rhizoma Chuanxiong 18K weight portion, Radix Rehmanniae Preparata 36K weight portion, for subsequent use.
By take Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) mixing, each once with 5 times amount 95% ethanol and 5 times amount 50% alcohol refluxs, each 2 hours, medicine juice filtered, and reclaimed ethanol, and filtration, filtrate is for subsequent use.
Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) three taste filtering residue and Radix Codonopsis, Poria, the Radix Paeoniae Alba, Radix Rehmanniae Preparata, Radix Glycyrrhizae Preparata 5 taste are decocted with water 2 times (Poria is decocted a drug wrapped), each 1.5 hours, amount of water is respectively 6 times, 4 times amount, and filter, merging filtrate is for subsequent use.
Merge above-mentioned filtrate, put single-effect external circulation concentrator or dual-effect concentrator and concentrate, solution to be concentrated relative density to 1.08-1.15 (50-75 DEG C), supernatant more than 48 hours.Get supernatant, filter, filtrate is for subsequent use.Above-mentioned filtrate is transferred to vacuum concentrator concentrate, makes the extractum that relative density is 1.35 ~ 1.38 (50 DEG C-60 DEG C heat are surveyed).
Above-mentioned extractum is divided into two equal portions, for subsequent use.
Embodiment 8
Preparation in the Example 7 and extractum that obtain is a, adding excipient is sucrose and appropriate dextrin, through granulating, drying, granulate, make granule 200K weight portion, be packaged into 8 weight portions/bag, obtain sugar-containing type BAZHEN KELI product.
Embodiment 9
Preparation in the Example 7 and extractum that obtain is a, adds appropriate soluble starch and appropriate acesulfame potassium, through granulating, drying, granulate, make granule 60K weight portion, be packaged into 3.5 weight portions/bag, obtain Sugarless type BAZHEN KELI product.
Embodiment 10
Take the prepared slices of Chinese crude drugs after concocting in embodiment 1 respectively, Radix Codonopsis 24K weight portion, Rhizoma Atractylodis Macrocephalae (parched) 24K weight portion, Poria 24K weight portion, Radix Glycyrrhizae Preparata 12K weight portion, Radix Angelicae Sinensis 36K weight portion, Radix Paeoniae Alba (parched) 24K weight portion, Rhizoma Chuanxiong 18K weight portion, Radix Rehmanniae Preparata 36K weight portion, add up to 198K weight portion, for subsequent use.According to the preparation method of the inventive method preparation and embodiment 2, be prepared into BAZHEN KELI extractum.Repetitive operation three batches.
According to the preparation method of open source literature and the preparation method of embodiment 7, preparation BAZHEN KELI extractum, repetitive operation three batches.
Above-mentioned BAZHEN KELI extractum weighs paeoniflorin content in total solid in extractum weight, extractum, wet extractum respectively, and its result is as following table 1.
Table 1 BAZHEN KELI extractum amount and paeoniflorin content result
From upper table 1 result, the inventive method and open source literature Measures compare, the extractum of extraction is converted to dry extract, on average reduces to 33.7K weight portion by 47.9K weight portion, decreases nearly 30%; And index composition peoniflorin extracted amount slightly increases.Illustrate that this aspect method can retain active ingredient preferably, reduce and extract extractum amount, thus solve the excessive problem of BAZHEN KELI open source literature method extraction extractum amount.
Embodiment 11
The BAZHEN KELI that Example 3, embodiment 4, embodiment 8, embodiment 9 are prepared from, place 6 months under temperature 40 DEG C ± 2 DEG C, relative humidity 75% ± 5% condition respectively, carry out accelerated stability test, respectively the 0th, sampling in 1,2,3,6 month, carry out quality testing.Measurement result is as following table 2:
Table 2 BAZHEN KELI accelerated stability test result
From stability test result, use the BAZHEN KELI (embodiment 3, embodiment 4) prepared of the inventive method when accelerated stability 6 months, its character does not change, and is not easy the moisture absorption; And BAZHEN KELI prepared by open source literature method (embodiment 8, embodiment 9) was when accelerated stability 6 months, character changes, and occurs slight caking phenomenon, also the easy moisture absorption, and its moisture is close to the maximum 6.0 of granule.
From result of the test, the BAZHEN KELI good stability using the inventive method to prepare is in the BAZHEN KELI using open source literature method to prepare.
Embodiment 12
Select Chinese medical discrimination to belong to the patient of deficiency of both QI and blood, the Clinical efficacy that BAZHEN KELI prepared by the BAZHEN KELI prepared by the technology of the present invention and open source literature method carries out the menoxenia for the treatment of deficiency of both QI and blood is tested.Sugarless type BAZHEN KELI prepared by Example 4(and the technology of the present invention), the Sugarless type BAZHEN KELI prepared of embodiment 9(and open source literature method) BAZHEN KELI that is prepared from, carry out the menoxenia clinical trial of QI and blood deficiency.
Deficiency of both QI and blood diagnostic criteria, cure mainly according to the function of BAZHEN KELI, disease feature, and to formulate with reference to " TCM syndrome diagosis therapeutics " (Beijing science tech publishing house), the guideline of clinical investigations of syndrome of deficiency of QI " new Chinese medicine treatment " (China Medical Science Press), " guideline of clinical investigations of new Chinese medicine treatment syndrome of deficiency of blood " (China Medical Science Press); Menoxenia diagnostic criteria is formulated with reference to " the clinical guidance principle of new Chinese medicine treatment menoxenia ".
Deficiency of both QI and blood therapeutic effect of syndrome evaluation criteria is formulated with reference to " guideline of clinical investigations of new Chinese medicine treatment syndrome of deficiency of QI ", " guideline of clinical investigations of new Chinese medicine treatment syndrome of deficiency of blood ".Clinical recovery: after treatment, clinical symptoms, sign disappear or substantially disappear, and syndrome integral reduces >=95%; Effective: after treatment, clinical symptoms, sign are obviously improved, syndrome integral reduces >=70%; Effective: after treatment, clinical symptoms, sign all take a favorable turn, syndrome integral reduces >=30%; Invalid: after treatment, symptom, sign are all not improved, even increase the weight of, syndrome integral reduces less than 30%.Computing formula (nimodipine method ([before (before treatment the rear integration of integration-treatment) ÷ treatment integration] × 100%.
Menoxenia the standard of curative effect evaluation is formulated with reference to " the clinical guidance principle of new Chinese medicine treatment menoxenia ".Clinical recovery: menstruation recovers normal, other transference cures through amount, menstrual period, integration minimizing >=95%; Effective: menstruation reduces 1/3 or be less than 100ml before amount comparatively treatment, and menstrual period replied within 7 days, other transference cures or alleviate, integration minimizing >=70%; Effective: through measuring, comparatively treating front improvement menstrual period after treatment, other symptoms alleviate before comparatively treating, and integration reduces >=30%; Invalid: after treatment through amount, menstrual period without improvement, integration reduce < 30%.
Instructions of taking: BAZHEN KELI prepared by BAZHEN KELI, open source literature method prepared by the technology of the present invention, is oral, each 1 bag, every day 2 times, takes 8 weeks continuously.
Result of the test is as follows:
Table 3 QIXUELIANGXU type therapeutic effect of syndrome compares
The above results adopts SPSS13.0 to carry out data analysis.Above-mentioned data input SPSS13.0 software, to number of cases weighting, 2 independent sample inspections of non parametric tests are adopted to carry out data analysis, from the known P=0.391 > 0.05 of data results, result of the test there was no significant difference is described, the BAZHEN KELI that namely prepared by the BAZHEN KELI prepared of the inventive method and open source literature method treats QI and blood deficiency syndrome therapeutic equivalence.
Table 4 menoxenia deficiency therapeutic effect of syndrome compares
The above results adopts SPSS13.0 to carry out data analysis.Above-mentioned data input SPSS13.0 software, to number of cases weighting, K independent sample inspection of non parametric tests is adopted to carry out data analysis, from the known P=0.518 > 0.05 of data results, result of the test there was no significant difference is described, it is suitable that the BAZHEN KELI that namely prepared by the BAZHEN KELI prepared of the inventive method and open source literature method treats menoxenia deficiency therapeutic effect of syndrome.
Claims (3)
1. low temperature extracts the method that binding film isolation technics prepares BAZHEN KELI continuously, it is characterized in that: preparation process comprises:
(1) BAZHEN KELI crude drug formula: Radix Codonopsis 50-70 weight portion, Rhizoma Atractylodis Macrocephalae (parched) 50-70 weight portion, Poria 50-70 weight portion, Radix Glycyrrhizae Preparata 20-40 weight portion, Radix Angelicae Sinensis 80-100 weight portion, Radix Paeoniae Alba (parched) 50-70 weight portion, Rhizoma Chuanxiong 40-50 weight portion, Radix Rehmanniae Preparata 80-100 weight portion;
(2) according to step (1) BAZHEN KELI crude drug formula, first take Radix Angelicae Sinensis wherein, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) mixing, open steam solvent preheater and start heating extraction solvent; Open solvent pump, heating after Extraction solvent---the ethanol injection of 70%-80% is in rotocel extractor, and Extraction solvent temperature controls at 60 ~ 65 DEG C, and solvent injection rate is 1950-2050L/h; Then open feeding system, put in rotocel extractor continuously by above-mentioned Radix Angelicae Sinensis, Rhizoma Chuanxiong, the mixed medical material of Rhizoma Atractylodis Macrocephalae (parched), it is 180-220kg/h that medical material drops into speed, and opens solvent circulating pump; Start to receive after the 1.5 ~ 2.0h that feeds intake and extract solution, extract solution and after filter, go to transfer storage tank by feed pump, enter enrichment process; After the 2.0h that feeds intake, open desolventizing machine concentrate extraction solution precipitation, the preliminary heating zone temperature of desolventizing machine controls at 80 ~ 90 DEG C, and zone of heating temperature controls at 90 ~ 100 DEG C, and baking zone temperature controls, at 90 ~ 100 DEG C, to obtain medicinal residues, and ethanol reclaims;
(3) the 3-4 times amount that added water by the filtering residue that the Radix Angelicae Sinensis of step (2) gained, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) are formed decocts 1.5-2 hour, filters and obtains the first filtrate, for subsequent use; All the other Radix Codonopsis, Poria, Radix Paeoniae Alba (parched), Radix Rehmanniae Preparata, Radix Glycyrrhizae Preparata 5 taste decoct with water 2 times according to after formula mixing, each 1-1.5 hour, amount of water is 5-6 times of above-mentioned 5 taste raw material tablets for the first time, second time amount of water is the 3-4 times amount of above-mentioned 5 taste raw material tablets, filter after decocting, the filtrate and the second filtrate that merge twice decoction are for subsequent use;
(4) combining step (3) two kinds of filtrates, select molecular weight cut off be 8000 ~ 12000 ultrafilter membrane carry out separation and purification, get ultrafiltration membrane permeate liquid, put in single-effect external circulation concentrator or the dense device of economic benefits and social benefits concentrated, during solution to be concentrated 85 DEG C, relative density stops concentrated to 1.10-1.15, clarify more than 24 hours, get supernatant; To be transferred to by above-mentioned supernatant in vacuum concentrator concentrated, when making 50 DEG C-60 DEG C, relative density is the extractum of 1.35 ~ 1.38;
(5) in the extractum of step (4), add excipient and/or correctives, through granulation, dry, granulate, make granule and obtain BAZHEN KELI product;
Excipient described in step (5) is at least one or two kinds and above mixture in sucrose, dextrin, soluble starch, starch, pregelatinized Starch.
2. low temperature according to claim 1 extracts the method that binding film isolation technics prepares BAZHEN KELI continuously, it is characterized in that: the BAZHEN KELI crude drug formula described in step (1): Radix Codonopsis 60 weight portion, Rhizoma Atractylodis Macrocephalae (parched) 60 weight portion, Poria 60 weight portion, Radix Glycyrrhizae Preparata 30 weight portion, Radix Angelicae Sinensis 90 weight portion, Radix Paeoniae Alba (parched) 60 weight portion, Rhizoma Chuanxiong 45 weight portion, Radix Rehmanniae Preparata 90 weight portion.
3. low temperature according to claim 1 extracts the method that binding film isolation technics prepares BAZHEN KELI continuously, it is characterized in that: the correctives described in step (5) is at least one in aspartame, stevioside, acesulfame potassium or two kinds and above mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310313541.5A CN103356801B (en) | 2013-07-23 | 2013-07-23 | Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310313541.5A CN103356801B (en) | 2013-07-23 | 2013-07-23 | Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103356801A CN103356801A (en) | 2013-10-23 |
| CN103356801B true CN103356801B (en) | 2015-02-11 |
Family
ID=49359603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310313541.5A Active CN103356801B (en) | 2013-07-23 | 2013-07-23 | Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103356801B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105878350A (en) * | 2016-04-12 | 2016-08-24 | 宁波立华制药有限公司 | Preparation method adopting low-temperature continuous extraction for Qixuekang oral liquid |
| CN105878351A (en) * | 2016-04-12 | 2016-08-24 | 宁波立华制药有限公司 | Preparation method of Qixuekang oral liquid |
| US10030000B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| EP3319949B1 (en) | 2016-09-21 | 2020-07-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| HUE047858T2 (en) | 2016-09-21 | 2020-05-28 | Celanese Int Corp | Acesulfame potassium compositions and processes for producing same |
| PL3319948T3 (en) | 2016-09-21 | 2021-12-27 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN106721738A (en) * | 2017-01-09 | 2017-05-31 | 吉林省轻工业设计研究院 | A kind of preparation technology of Black Box Tracing health drink |
| CN107441465A (en) * | 2017-07-19 | 2017-12-08 | 孙凌飞 | Purification solution based on ancient prescription draft conditioning skin prepares and its application of derivative |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068468A (en) * | 2009-12-31 | 2011-05-25 | 成都科尔医药技术有限公司 | Method for treating traditional Chinese medicinal extraction solution before preparation |
| CN102441291A (en) * | 2011-12-01 | 2012-05-09 | 吉林省包装工程研究中心 | New method for extracting or purifying effective component of traditional Chinese medicine |
| CN202777089U (en) * | 2012-09-21 | 2013-03-13 | 南京中医药大学 | Multifunctional traditional Chinese medicine extracting, refining and concentrating equipment |
| CN103127741A (en) * | 2013-02-20 | 2013-06-05 | 中国科学院过程工程研究所 | Method for enhancing natural product solvent extraction through membrane separation process |
-
2013
- 2013-07-23 CN CN201310313541.5A patent/CN103356801B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068468A (en) * | 2009-12-31 | 2011-05-25 | 成都科尔医药技术有限公司 | Method for treating traditional Chinese medicinal extraction solution before preparation |
| CN102441291A (en) * | 2011-12-01 | 2012-05-09 | 吉林省包装工程研究中心 | New method for extracting or purifying effective component of traditional Chinese medicine |
| CN202777089U (en) * | 2012-09-21 | 2013-03-13 | 南京中医药大学 | Multifunctional traditional Chinese medicine extracting, refining and concentrating equipment |
| CN103127741A (en) * | 2013-02-20 | 2013-06-05 | 中国科学院过程工程研究所 | Method for enhancing natural product solvent extraction through membrane separation process |
Non-Patent Citations (2)
| Title |
|---|
| 华耀祖.超滤在中药中的应用.《膜分离技术与应用丛书》.化学工业出版社,2004,423-426. * |
| 吴清.八珍颗粒.《230种中药颗粒剂和胶囊剂制备关键技术》.化学工业出版社,2009,29-30. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103356801A (en) | 2013-10-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103356801B (en) | Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology | |
| CN103041100A (en) | Traditional Chinese medicine preparation for treatment of hypomenorrhea and preparation method thereof | |
| CN103191298B (en) | Traditional Chinese medicinal composition for treating blood group incompatibility haemolytic disease and preparation method thereof | |
| CN103349707B (en) | Method for preparing eight-treasure granules | |
| CN106390048A (en) | Extraction method for Xiaochaihu decoction and radix bupleuri-dragon's bone-oyster decoction | |
| CN104758736A (en) | Blood-glucose-reducing traditional Chinese medicine composition and preparation method thereof | |
| CN103099788A (en) | Traditional Chinese medicine composite decoration from powder, preparation and decoction methods and dosage relation thereof | |
| CN102920964A (en) | Traditional Chinese medicine preparation for curing cough | |
| CN100500183C (en) | Preparation of Chinese medicinal mixture for treating gynecologic menstrual disease | |
| CN103784771A (en) | Traditional Chinese medicine composition has functions of anticoccidia, haemostasis and blood enriching, and antibiosis and antiphlogosis, and preparation method thereof | |
| CN1840134A (en) | Capsule for treating climacteric syndrome | |
| CN104524273A (en) | Preparation method of Yinqiao preparation | |
| CN101224283A (en) | Chinese traditional medicine compounds for treating diabetes and preparing method thereof | |
| CN108686094B (en) | Traditional Chinese medicine for reducing blood sugar and preparation method thereof | |
| CN107669726A (en) | Treat the wormwood extract liniment of eczema | |
| CN109172729B (en) | Lung-clearing paste and preparation method thereof | |
| CN102233089B (en) | Traditional Chinese medicine composition and preparation method thereof | |
| CN102580042A (en) | Traditional Chinese medicine composition for treating wind-cold type of common cold and preparation method of traditional Chinese medicine composition | |
| CN101461877B (en) | Medicament composition for recovery of physical strength for women | |
| CN104771595A (en) | Chinese medicinal composition for enhancing immunity and preparation method thereof | |
| CN110960646A (en) | Preparation method of Yunkang oral liquid | |
| CN115252729B (en) | Traditional Chinese medicine composition for treating diabetes and application thereof | |
| CN114796417B (en) | Blood sugar reducing traditional Chinese medicine formula and preparation method thereof | |
| CN102488851A (en) | Drug for treating recurrent genital herpes and preparation method thereof | |
| CN106421306A (en) | Anemarrhenae, phellodendrom and rehmannia pill |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Jiang Hailong Inventor after: Sun Zhenjiao Inventor after: Zhou Haibin Inventor after: Wang Jun Inventor after: Feng Dingjun Inventor after: Yu Wei Inventor after: Liu Bangmin Inventor before: Feng Dingjun Inventor before: Sun Zhenjiao Inventor before: Wang Jun Inventor before: Jiang Hailong Inventor before: Yu Wei Inventor before: Lu Yujiang |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: FENG DINGJUN SUN ZHENJIAO WANG JUN JIANG HAILONG YU WEI LU YUJIANG TO: JIANG HAILONG SUN ZHENJIAO ZHOU HAIBIN WANG JUN FENG DINGJUN YU WEI LIU BANGMIN |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder |
Address after: 315174 Xinlian village, Gaoqiao Town, Haishu District, Ningbo City, Zhejiang Province Patentee after: NINGBO LIWAH PHARMACEUTICAL Co.,Ltd. Address before: 315174 New Union Village, Gaoqiao Town, Yinzhou District, Ningbo, Zhejiang Patentee before: NINGBO LIWAH PHARMACEUTICAL Co.,Ltd. |
|
| CP02 | Change in the address of a patent holder |