CN104771714A - Mulberry ginger extract and preparation process and application thereof - Google Patents
Mulberry ginger extract and preparation process and application thereof Download PDFInfo
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- CN104771714A CN104771714A CN201410017162.6A CN201410017162A CN104771714A CN 104771714 A CN104771714 A CN 104771714A CN 201410017162 A CN201410017162 A CN 201410017162A CN 104771714 A CN104771714 A CN 104771714A
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- rhizoma zingiberis
- zingiberis recens
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Abstract
The invention relates to a mulberry ginger extract and a preparation process and an application thereof. The mulberry ginger extract comprises the formula by weight: 30 parts of mulberry leaves, 16 parts of fructus forsythiae, 12 parts of chrysanthemum, 10 parts of dried ginger, 16 parts of semen armeniacae amarae, and 16 parts of folia perillae acutae. The invention provides the mulberry ginger extract preparation process which can greatly shorten the production cycle, improves phillyrin transfer rate and removes impurities.
Description
Technical field
The invention belongs to compound Chinese medicinal preparation field, particularly a kind of Mulberry Rhizoma Zingiberis Recens extractum, preparation technology and application thereof.
Background technology
Need to extract six kinds of compositions (Folium Mori, Flos Chrysanthemi, Fructus Forsythiae, Semen Armeniacae Amarum, Rhizoma Zingiberis, Folium Perillae) of Sang Jiangzhong in the preparation process of Mulberry Rhizoma Zingiberis Recens, finally obtain Mulberry Rhizoma Zingiberis Recens extractum, then produce the products such as mulberry leaf-ginger common cold sheet, mulberry leaf-ginger common cold capsule, mulberry leaf-ginger common cold injection as required.These products all have effect of loose wind heat clearing away, expelling phlegm for arresting cough, are mainly used in treatment flu, cough, headache, laryngopharynx swelling and pain.
In large batch of extracting technique of Chinese medicine is produced, employing be decoction and alcohol sedimentation technique, but, in long-term use procedure, find to there is many problems: the first, can not unavoidably impurity be extracted during water extraction.Second, precipitate with ethanol remove impurity, aminoacid in effective ingredient, polysaccharide etc. are insoluble to ethanol and can be removed, although alkaloid, glycosides, flavonoid are dissolved in ethanol, but there will be in the operating process of remove impurity in various degree wrap up in phenomenon, cause natively few effective ingredient to lose again, thus affect the clinical efficacy of Chinese medicine preparation.3rd, production cost is high, and in the removal process of ethanol, consumption alcohol amount is large.4th, the drug effect of finished product is poor, and stability is low, and in repeatedly precipitate with ethanol process, the loss of effective ingredient is large.
Adsorption clarification adds a kind of absorptive clarificant in Chinese medicine extraction liquid or extracting solution concentrated solution, removed the coarse granule in solution by the mode of absorption, reaches refining and a new and high technology of raising preparation clarity object.And the absorptive clarificant used be a kind of by absorption, build bridge, flocculation and inorganic salt electrolyte particulates and surface charge produce cohesion etc., make the larger granule of granularity in system and there is the flocculate suspended particles precipitation of stoke precipitation trend.
At present, have no and prepare Mulberry Rhizoma Zingiberis Recens extractum and the report to this Mulberry Rhizoma Zingiberis Recens extractum application about combining with adsorption clarification.
Summary of the invention
The object of the invention is to provide a kind of Mulberry Rhizoma Zingiberis Recens extractum.
Meanwhile, the present invention also aims to the preparation technology that a kind of Mulberry Rhizoma Zingiberis Recens extractum is provided.
Further, the present invention also aims to provide the application of a kind of Mulberry Rhizoma Zingiberis Recens extractum in compound Chinese medicinal preparation.
The preparation technology of Mulberry Rhizoma Zingiberis Recens extractum of the present invention comprises the steps:
(1) take Folium Mori, Fructus Forsythiae, Flos Chrysanthemi, Fructus Forsythiae, Semen Armeniacae Amarum, Folium Perillae by Mulberry Rhizoma Zingiberis Recens formula proportion, will after the Six-element Chinese crude drug co-grinding weighed up, add the 3-10 water doubly of medical material weight, and soak 1-3 hour;
(2) the wet medical material obtained in step (1) is put into extraction vessel together with its soak, extract, obtain extracting solution;
(3) add natural clarifying agent in the extracting solution obtained to step (2), stir, temperature remains on 25-85 DEG C, leaves standstill after 1-8 hour, filters, and gets filtrate concentrating, obtains Mulberry Rhizoma Zingiberis Recens extractum I;
(4) supernatant obtained in step (3) is carried out microporous filter, get Sang Jiang filtrate;
(5) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (4), obtains the Mulberry Rhizoma Zingiberis Recens extractum needed for production;
In Mulberry Rhizoma Zingiberis Recens formula described in step (1), composition by weight: 30 parts, Folium Mori, Fructus Forsythiae 16 parts, Flos Chrysanthemi 12 parts, Rhizoma Zingiberis 10 parts, Semen Armeniacae Amarum 16 parts, Folium Perillae 16 parts
Amount of water described in step (1), preferably the 3-6 of medical material gross weight doubly.
Extraction described in step (2), extraction time is 1-4 time, and further decocting extraction time is 2-8 hour.
Natural clarifying agent described in step (3) is the one in chitosan, fruit juice 101 or ZTC1+1 II type, preferably ZTC1+1 II type natural clarifying agent.
Natural clarifying agent described in step (3) is ZTC1+1 II type natural clarifying agent, 2%-10% and 4%-20% that wherein composition is A, the addition sequence of B component is A after first B, further A, B component addition is respectively medicine liquid volume.
Natural clarifying agent described in step (3), be ZTC1+1 II type natural clarifying agent, A, B component are made into A, the B solution of 1% respectively with 1% acetic acid according to operation instruction.
The aperture of the micropore filtering film described in step (4) is 1.2 μm.
Add ethanol in proper amount or water standing 5-24 hour precipitation further after preferred steps (3), get supernatant.
Preferably, the supernatant obtained after adding alcohol settling after described step (3) continues to add water and staticly settles further, obtains supernatant.
According to need of production, by the Mulberry Rhizoma Zingiberis Recens extractum of preparation, be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens granule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
ZTC1+1 type natural clarifying agent used in foregoing is produced by Beijing Zheng Tiancheng clarification technique company limited and is provided.
The present invention adopts and extracts above-mentioned Six-element Chinese crude drug, adsorption clarification technology is used in the process of remove impurity, natural clarifying agent is added in extracting solution, finally also use water precipitating and Millipore filtration techniques to the further remove impurity of extracting solution, ensure that the quality of effective ingredient in the efficient removing of few residual, the impurity of natural clarifying agent in extracting solution and extracting solution.Application adsorption clarification technology and alcohol settling, water precipitation combines and prepares the process of Mulberry Rhizoma Zingiberis Recens extractum, simplifies production technology, shortens the production time, instead of traditional ethanol remove impurity with natural clarifying agent, cost-saving, avoids the environmental pollution that ethanol brings.Apply Mulberry Rhizoma Zingiberis Recens preparation prepared by Mulberry Rhizoma Zingiberis Recens extractum prepared by this production technology and there is good market prospect.
Detailed description of the invention
Embodiment 1
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, take Folium Mori 30kg, Fructus Forsythiae 16kg, Flos Chrysanthemi 12kg, Rhizoma Zingiberis 10kg, Semen Armeniacae Amarum 16kg, Folium Perillae 16kg, 3 times of water yields of medical material weight will be added after Six-element Chinese crude drug co-grinding, soak 3 hours;
(2) wet medical material step (1) obtained, together with its soak, puts into Chinese medicine extracting tank, decocts 6 hours, decocts 2 times, filters, merges 2 extracting solution;
(3) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 4% is added in the extracting solution obtained to step (2), stir, after fluid temperature is raised to 65 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 2%, stir, leave standstill after 8 hours, filter, filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum I;
(4) add 1 times of volume 70% ethanol in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (3) to dissolve completely to extractum, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(5) supernatant obtained in step (4) is carried out the microporous filter of 1.2 μm, get Sang Jiang filtrate;
(6) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (5), get Sang Jiang extractum;
(7) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (6), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens granule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
Embodiment 2
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, taking Folium Mori 15kg, Fructus Forsythiae 8kg, Flos Chrysanthemi 6kg, Rhizoma Zingiberis 5kg, Semen Armeniacae Amarum 8kg, Folium Perillae 8kg, by adding 10 times of water yields of medical material weight own after the Six-element Chinese crude drug co-grinding weighed up, soaking 3 hours;
(2) wet medical material step (1) obtained, together with its soak, puts into Chinese medicine extracting tank, decocts 2 hours, decocts 4 times, filters, merge extractive liquid;
(3) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 20% is added in the extracting solution obtained to step (2), stir, after fluid temperature is raised to 85 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 10%, stir, leave standstill after 1 hour, filter, filtrate concentrates, and obtains Mulberry Rhizoma Zingiberis Recens extractum I;
(4) add 2 times of volume 60% ethanol in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (3) to dissolve completely to extractum, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(5) supernatant obtained in step (4) is carried out the microporous filter of 1.2 μm, get Sang Jiang filtrate;
(6) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (5), get Sang Jiang extractum;
(7) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (6), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens granule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
Embodiment 3
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, take Folium Mori 15kg, Fructus Forsythiae 8kg, Flos Chrysanthemi 6kg, Rhizoma Zingiberis 5kg, Semen Armeniacae Amarum 8kg, Folium Perillae 8kg, 6 times of water gagings of medical material weight will be added after Six-element Chinese crude drug co-grinding, soak 1 hour;
(2) wet medical material step (1) obtained, together with its soak, puts into Chinese medicine extracting tank, decocts 8 hours, decocts 2 times, filters, merge extractive liquid;
(3) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 8% is added in the extracting solution obtained to step (2), stir, after fluid temperature is raised to 70 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 4%, stir, leave standstill after 3 hours, filter, filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum;
(4) add 2 times of volume ethanol in the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (3) to dissolve completely to extractum, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(5) supernatant obtained in step (4) is carried out the microporous filter of 1.2 μm, get Sang Jiang filtrate;
(6) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (5), get Sang Jiang extractum;
(7) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (6), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens granule, Mulberry Rhizoma Zingiberis Recens capsule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
Embodiment 4
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, take Folium Mori 30kg, Fructus Forsythiae 16kg, Flos Chrysanthemi 12kg, Rhizoma Zingiberis 10kg, Semen Armeniacae Amarum 16kg, Folium Perillae 16kg, 5 times of water gagings of medical material weight will be added after Six-element Chinese crude drug co-grinding, soak 2 hours;
(2) wet medical material step (1) obtained, together with its soak, puts into Chinese medicine extracting tank, decocts 8 hours, decocts 2 times, filters, merges 2 extracting solution;
(3) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 10% is added in the extracting solution obtained to step (2), stir, after fluid temperature remains on 25 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 5%, stir, leave standstill after 8 hours, filter, filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum I;
(4) add 2 times of volume 70% ethanol in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (3) and leave standstill 10 hours, filter and obtain supernatant, concentrated, then add 0.5 times of volume distilled water, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(5) supernatant obtained in step (4) is carried out the microporous filter of 1.2 μm, get Sang Jiang filtrate;
(6) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (5), get Sang Jiang extractum;
(7) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (6), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens granule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
Embodiment 5
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, take Folium Mori 15kg, Fructus Forsythiae 8kg, Flos Chrysanthemi 6kg, Rhizoma Zingiberis 5kg, Semen Armeniacae Amarum 8kg, Folium Perillae 8kg, 3 times of water yields of medical material weight will be added after Six-element Chinese crude drug co-grinding, soak 2 hours;
(2) wet medical material step (1) obtained, together with its soak, puts into Chinese medicine extracting tank, decocts 5 hours, decocts 4 times, filters, merges 4 extracting solution;
(3) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 16% is added in the extracting solution obtained to step (2), stir, after fluid temperature is raised to 50 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 8%, stir, leave standstill after 6 hours, filter, filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum I;
(4) add 1 times of 80% ethanol in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (3) and leave standstill 12 hours, filter and obtain supernatant, concentrated, then add 1 times of volume distilled water, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(5) supernatant obtained in step (4) is carried out the microporous filter of 1.2 μm, get Sang Jiang filtrate;
(6) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (5), get Sang Jiang extractum;
(7) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (6), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens granule, Mulberry Rhizoma Zingiberis Recens capsule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
Embodiment 6
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, take Folium Mori 30kg, Fructus Forsythiae 16kg, Flos Chrysanthemi 12kg, Rhizoma Zingiberis 10kg, Semen Armeniacae Amarum 16kg, Folium Perillae 16kg, 6 times of water yields of medical material weight will be added after Six-element Chinese crude drug co-grinding, soak 2 hours;
(2) wet medical material step (1) obtained, together with its soak, puts into Chinese medicine extracting tank, decocts 6 hours, decocts 2 times, filters, merge extractive liquid;
(3) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 10% is added in the extracting solution obtained to step (2), stir, after fluid temperature is raised to 85 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 5%, stir, leave standstill after 7 hours, filter, filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum I;
(4) add 1 times of 90% ethanol in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (3) and leave standstill 10 hours, filter and obtain supernatant, concentrated, then add 1 times of volume distilled water, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(5) supernatant obtained in step (4) is carried out the microporous filter of 1.2 μm, get Sang Jiang filtrate;
(6) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (5), get Sang Jiang extractum;
(7) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (6), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens granule, Mulberry Rhizoma Zingiberis Recens capsule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
Comparative Examples 1
(1) get Folium Mori 30kg, Fructus Forsythiae 16kg, Flos Chrysanthemi 12kg, Rhizoma Zingiberis 10kg, Semen Armeniacae Amarum 16kg, Folium Perillae 16kg, and slightly pulverized by Six-element medical material, decoct with water three times, 2 hours first times, second and third time each 1 hour, collecting decoction, filters, get Sang Jiang Aqueous extracts;
(2) the Mulberry Rhizoma Zingiberis Recens Aqueous extracts will obtained in step (1), leaves standstill a period of time, filters, and filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum I;
(3) add distilled water in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (2) to dissolve completely to extractum, leave standstill 24 hours, high speed centrifugation, gets supernatant concentration, obtains Mulberry Rhizoma Zingiberis Recens cream for subsequent use;
(4) according to production is required can with the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (3), in addition adjuvant accordingly, and carry out corresponding technical process, can obtain Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens granule, Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection etc.
Comparative Examples 2
(1) by Mulberry Rhizoma Zingiberis Recens formula proportion, get 15kg powder of Folium Mori and be broken into fine powder, residue 15kg Folium Mori and all the other gomi herbs (Fructus Forsythiae 16kg, Flos Chrysanthemi 12kg, Rhizoma Zingiberis 10kg, Semen Armeniacae Amarum 16kg, Folium Perillae 16kg) decoct with water three times, 2 hours first times, second and third time each 1 hour, collecting decoction, filters, get Sang Jiang Aqueous extracts;
(2) add ethanol in the Mulberry Rhizoma Zingiberis Recens Aqueous extracts obtained in step (1), make alcohol content be 60%, 70%, 80%, leave standstill, filter, get filtrate, concentration and recovery ethanol, obtain Mulberry Rhizoma Zingiberis Recens extractum I;
(3) add distilled water in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (2) to dissolve completely to extractum, leave standstill 24 hours, by medicinal liquid high speed centrifugation, get supernatant, the concentrated Mulberry Rhizoma Zingiberis Recens extractum obtaining need of production;
(4) obtain get Sang Jiang extractum with in step (3), with Folium Mori fine powder for carrier, add corresponding adjuvant, then combine with certain production technology, prepare the Mulberry Rhizoma Zingiberis Recens dosage form (Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens granule) required for production.
Comparative Examples 3
(1) Folium Mori 30kg is taken, Fructus Forsythiae 16kg, Flos Chrysanthemi 12kg, Rhizoma Zingiberis 10kg, Semen Armeniacae Amarum 16kg, Folium Perillae 16kg, after slightly being pulverized by Six-element medical material, decocts with water three times, 2 hours first times, second and third time each 1 hour, collecting decoction, filters, obtain Mulberry Rhizoma Zingiberis Recens Aqueous extracts;
(2) the B component solution of natural clarifying agent ZTC1+1 II type of medicine liquid volume 10% is added in the Mulberry Rhizoma Zingiberis Recens Aqueous extracts obtained to step (1), stir, after fluid temperature is raised to 75 DEG C, add the component A solution of ZTC1+1 II type of medicine liquid volume 5%, stir, leave standstill after 7 hours, filter, filtrate carries out concentrated obtaining Mulberry Rhizoma Zingiberis Recens extractum I;
(3) add distilled water in the Mulberry Rhizoma Zingiberis Recens extractum I obtained in step (2) to dissolve completely to extractum, leave standstill 24 hours, high speed centrifugation, gets supernatant;
(4) supernatant obtained in concentration step (3), get Sang Jiang extractum;
(5) according to need of production, utilize the Mulberry Rhizoma Zingiberis Recens extractum obtained in step (4), be equipped with suitable adjuvant, then pass through corresponding technical process, obtained Mulberry Rhizoma Zingiberis Recens tablet, Mulberry Rhizoma Zingiberis Recens granule, Mulberry Rhizoma Zingiberis Recens capsule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
The screening of experimental example 1 natural clarifying agent of the present invention
1. instrument and reagent:
Ultraviolet spectrophotometer; Electronic balance (ten thousand/); High speed centrifuge; Multifunctional extracting pot; Chitosan; Fruit juice 101; ZTC1+1 II type natural clarifying agent.
2. method and result
The preparation of 2.1 Mulberry Rhizoma Zingiberis Recens extracting solution
(1) take Folium Mori 30g by formula, Fructus Forsythiae 16g, Flos Chrysanthemi 12g, Rhizoma Zingiberis 10g, Semen Armeniacae Amarum 16g, Folium Perillae 16g, the 6 times amount water soaking 2 hours of medical material weight will be added after Six-element Chinese crude drug co-grinding,
(2) the wet medical material obtained in step (1) is extracted 3 times together with its soak, merge three extracting solution, obtain Mulberry Rhizoma Zingiberis Recens extracting solution.
The preparation of 2.2 clarifiers
(1) preparation of chitosan solution: take appropriate Chitosan powder, the acetum with 1% be mixed with containing 1% chitosan 1% acetum.
(2) preparation of fruit juice 101 solution: take appropriate fruit juice 101 powder, the acetum with 1% be mixed with containing 1% fruit juice 101 1% acetum.
(3) preparation of ZTC1+1 II type clarifier: take the component A powder in appropriate ZTC1+1 II type, 1%A component solution is made into 1% acetic acid, namely first use a small amount of 1% acetate dissolution, fully stir, after viscose to be formed, add swelling 24 hours of 1% acetum of amount of calculation again.The solution of 1%B component is made in the same way with 1% acetic acid.
2.3 clarifying process
(1) get three parts of above-mentioned Mulberry Rhizoma Zingiberis Recens extracting solution 50ml, be numbered I, II, III.
(2) in the Mulberry Rhizoma Zingiberis Recens extracting solution being numbered I, add the chitosan solution prepared of 10%; 10% fruit juice 101 solution is added in numbering II; First add 10%B component solution in numbering III, after stirring, then add 5%A component solution.
(3) three groups of sample temperatures are remained on 50 DEG C, leave standstill after 6 hours, observe flco situation, high speed centrifugation, gets the supernatant of three groups of samples.
(4) with the light transmittance of uv-spectrophotometric note detection three groups of supernatant, and result is recorded.
2.4 experimental results are as shown in table 1
| Numbering I | Numbering II | Numbering III | |
| Flco situation | Fine granularity, thread | Thread | Thread, little cotton-shaped |
| Light transmittance (%) | 64 | 55 | 70 |
Shown by result in table, under equal conditions remove the impurity in Mulberry Rhizoma Zingiberis Recens extracting solution, select natural clarifying agent ZTC1+1 II best.
Experimental example 2 uses the conditional filtering of clarifier ZTC1+1 II type remove impurity
1. instrument and reagent
Controllable temperature water-bath, high speed centrifuge, ZTC1+1 II type clarifier
2. method and result
When carrying out purification with clarifier to Mulberry Rhizoma Zingiberis Recens extracting solution, the effective ingredient affected in Mulberry Rhizoma Zingiberis Recens extracting solution has the factors such as temperature, time, clarifier addition, and this experiment investigates the clarifier temperature of ZTC1+1 II type when carrying out adsorption and the addition of clarifier emphatically.
The investigation of 2.1 additions
(1) get the Mulberry Rhizoma Zingiberis Recens extracting solution that 5 parts of volumes are identical, be numbered A
1, A
2, A
3, A
4, A
5, be all put in the thermostat water bath of identical temperature.
(2) to being numbered A
1, A
2, A
3, A
4, A
5the middle B component solution adding 2%, 4%, 8%, 16%, 20% ZTC1+1 configured II type of medicine liquid volume respectively, (addition is the half of corresponding B component solution to add the component A solution prepared after stirring respectively, namely 1%, 2%, 4%, 8%, 10%), leave standstill after 6 hours, observe solution conditions.
(3) experimental result is as table 2:
| A 1（2%） | A 2（4%） | A 3（8%） | A 4（16%） | A 5（20%） | |
| Solution conditions | Brown muddiness | Brown more muddy | Dark-brown is transparent | Dark-brown is transparent | Dark-brown is transparent |
| Sedimentation situation | Sedimentation is incomplete | Precipitation not exclusively | Sedimentation is complete | Sedimentation is complete | Sedimentation is complete |
Note: the percent in bracket is the addition of B component solution in ZTC1+1 II type natural clarifying agent
Drawn by the phenomenon result in table 2, in ZTC1+1 II type, the addition optimum of B component is 8%-16%.
The investigation of 2.2 temperature
(1) get the Mulberry Rhizoma Zingiberis Recens extracting solution that 5 parts of volumes are identical, be numbered B
1, B
2, B
3, B
4, B
5.
(2) respectively 5 parts of Mulberry Rhizoma Zingiberis Recens extracting solution are put into the water-bath that temperature is 40 DEG C, 50 DEG C, 65 DEG C, 75 DEG C, 85 DEG C, the B component solution of mutually commensurability ZTC1+1 II type clarifier is added in five groups of samples, after stirring, add component A solution again, leave standstill after 6 hours, observe sample solution situation.
(3) experimental result is as table 3:
| B 1（40℃） | B 2（50℃） | B 3（65℃） | B 4（75℃） | B 5（85℃） | |
| Precipitate morphology | A small amount of graininess | Graininess | Graininess, little cotton-shaped | Cotton-shaped | Cotton-shaped |
| Sedimentation situation | Precipitation not exclusively | Precipitation not exclusively | Precipitation completely | Precipitation completely | Precipitation completely |
Drawn by the phenomenon result in table 3, use ZTC1+1 II type natural clarifying agent to carry out the optimum temperature range of adsorption clarification for 65-85 DEG C to Mulberry Rhizoma Zingiberis Recens extracting solution.
Experimental example 3 adsorption clarification technology compares with the clearance of the protein of traditional precipitate with ethanol technology
1. this experimental example passes through two kinds of technology the judge index of the clearance of the protein in Mulberry Rhizoma Zingiberis Recens extracting solution as two kinds of technology qualities.
2. instrument and reagent
Electronic balance, visible ultraviolet spectrophotometer, bovine serum albumin (BSA), Coomassie brilliant G-250
3. method and result
The preparation of 3.1 developers
Take Coomassie brilliant G-250 100mg, add 50ml95% ethanol, after dissolving, add 100ml85%(w/v again) H
3pO
4, be adjusted to 1000ml with distilled water, be Coomassie brilliant blue working solution.
The preparation of 3.2 standard curves
3.2.1 the preparation of titer
(1) get bovine serum albumin (BSA) to be dissolved in right amount in 10ml distilled water.
(2) draw bovine serum albumin stock solution 0ml, 0.1ml, 0.2ml, 0.8ml, 1.4ml, 2.0ml, 2.6ml, 3.0ml respectively in 8 10ml tool plug test tubes, add 5ml Coomassie brilliant blue working solution, finally supplement distilled water to 10ml, mixing.
3.2.2 the drafting of standard curve
By Specification Curve of Increasing method, recording absorbance at 595nm place, take absorbance A as vertical coordinate, and concentration C (ug/ml) is abscissa, and result is as table 4:
Equation of linear regression is: A=0.0007C-0.0036.
Correlation coefficient: R=0.9997
The preparation of 3.3 need testing solutions
Draw unpurified Mulberry Rhizoma Zingiberis Recens extracting solution and the extracting solution 0.1ml after clarifying adsorption treatment in above-described embodiment 1-6 and Comparative Examples 1-4 respectively and be placed in 10ml tool plug test tube, add 5ml Coomassie Brillant Blue solution, add water to 10ml.Obtain need testing solution.
3.4 methods and result
Under wavelength 595nm, record the absorbance of need testing solution successively, calculate protein removal rate, result is as table 5:
| Protein removal rate (%) | |
| Embodiment 1 | 88.9 |
| Embodiment 2 | 90.6 |
| Embodiment 3 | 92.0 |
| Embodiment 4 | 91.9 |
| Embodiment 5 | 90.3 |
| Embodiment 6 | 94.6 |
| Comparative Examples 1 | 43.5 |
| Comparative Examples 2 | 73.2 |
| Comparative Examples 3 | 81.3 |
Shown by result in table 5, use clarification adsorption technology to carry out purification to Mulberry Rhizoma Zingiberis Recens extracting solution, substantially increase the clearance of protein.
Experimental example 4 prepares the traditional handicraft of Mulberry Rhizoma Zingiberis Recens extractum and the technics comparing after improving
1. this experimental example is by comparing the traditional handicraft of preparation Mulberry Rhizoma Zingiberis Recens extractum and the technique after improving as judge index the rate of transform of Determination of forsythin contained in Mulberry Rhizoma Zingiberis Recens extractum and phillyrin.
2. instrument and reagent
Reagent used in this experiment is not marked is all analytical pure, and water used is ultra-pure water.
High performance liquid chromatograph, acetonitrile (chromatographically pure), methanol, petroleum ether, Fructus Forsythiae medical material (Fructus Forsythiae used with preparation Mulberry Rhizoma Zingiberis Recens extractum belongs to same batch)
3. method and result
The preparation of 3.1 phillyrin reference substance solution
It is appropriate that precision takes phillyrin reference substance, adds methanol and make the solution of every 1ml containing 0.2mg phillyrin, obtain phillyrin reference substance solution.
The preparation of 3.2 Fructus Forsythiae Authentic plant drugs solution
By appropriate Fructus Forsythiae pulverizing medicinal materials, accurately take Weeping Forsythia Capsule 1g, add petroleum ether (30 DEG C-60 DEG C) 40ml, supersound process 30 minutes, filter, discard petroleum ether liquid, volatilize, 40ml methanol is added in residue, supersound process 40 minutes, filters, filtrate evaporate to dryness, residue adds methanol 4ml makes dissolving, as Fructus Forsythiae Authentic plant drugs solution.
The preparation of 3.3 need testing solutions
(1) get the Mulberry Rhizoma Zingiberis Recens extractum that appropriate above-described embodiment 1-6 and Comparative Examples 1-4 is obtained respectively, be concentrated into Mulberry Rhizoma Zingiberis Recens dry extract further;
(2) take the Mulberry Rhizoma Zingiberis Recens dry extract 0.5g obtained in step (1) respectively, add proper amount of methanol and dissolve and be settled to 25ml, be i.e. get Sang Jiang need testing solution.
3.4HPLC method measures the Determination of forsythin in two groups of need testing solutions
Be filler with octadecylsilane chemically bonded silica, acetonitrile-water (25:75) is mobile phase, determined wavelength is under the chromatographic condition of 277nm, with 10 μ l for sample size, carry out detection to the above-mentioned need testing solution prepared successively to analyze, theoretical cam curve is pressed phillyrin peak and is calculated, and should be not less than 3000.
3.5 testing results are as table 6:
Determination of forsythin in the Fructus Forsythiae Authentic plant drugs solution finally recorded is 6.31mg/g.
| The rate of transform (%) | |
| Embodiment 1 | 83.5 |
| Embodiment 2 | 81.4 |
| Embodiment 3 | 82.0 |
| Embodiment 4 | 82.2 |
| Embodiment 5 | 85.9 |
| Embodiment 6 | 90.2 |
| Comparative Examples 1 | 51.4 |
| Comparative Examples 2 | 52.3 |
| Comparative Examples 3 | 63.1 |
Can be drawn by the data in table 6, the Mulberry Rhizoma Zingiberis Recens extractum prepared by method of the present invention, compared with traditional handicraft, the rate of transform of phillyrin improves greatly.
In sum, the preparation technology of a kind of Mulberry Rhizoma Zingiberis Recens extractum of the present invention, substantially reduces the production cycle, improves the rate of transform of phillyrin, the quality of Mulberry Rhizoma Zingiberis Recens extractum of the present invention is improved greatly, and then improves the drug effect being further processed into and producing upper required preparation type.
Claims (10)
1. a Mulberry Rhizoma Zingiberis Recens extractum, is characterized in that the Chinese medicine formula (by weight) of described preparation Mulberry Rhizoma Zingiberis Recens extractum is 30 parts, Folium Mori, Fructus Forsythiae 16 parts, Flos Chrysanthemi 12 parts, Rhizoma Zingiberis 10 parts, Semen Armeniacae Amarum 16 parts, Folium Perillae 16 parts; Extractum adopts natural clarifying agent to carry out remove impurity.
2., according to a kind of Mulberry Rhizoma Zingiberis Recens extractum described in claim 1, it is characterized in that preparation technology comprises the following steps:
(1) get Folium Mori, Fructus Forsythiae, the Flos Chrysanthemi by Mulberry Rhizoma Zingiberis Recens formula proportion, Rhizoma Zingiberis, Semen Armeniacae Amarum, Folium Perillae, the 3-10 water doubly of medical material weight will be added after Six-element Chinese crude drug co-grinding, and soak 1-3 hour;
(2) the wet medical material obtained in step (1) is loaded in extraction vessel together with its soak, extract, obtain extracting solution;
(3) add natural clarifying agent in the merge extractive liquid, obtained to step (2), stir, temperature remains on 25-85 DEG C, and leave standstill after 1-8 hour, high speed centrifugation, gets supernatant;
(4) supernatant obtained in step (3) is carried out microporous filter, get Sang Jiang filtrate;
(5) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (4), get Sang Jiang extractum.
3. according to the preparation method of a kind of Mulberry Rhizoma Zingiberis Recens extractum described in claim 1 be: (1) gets Folium Mori, Fructus Forsythiae, Flos Chrysanthemi by Mulberry Rhizoma Zingiberis Recens formula proportion, Rhizoma Zingiberis, Semen Armeniacae Amarum, Folium Perillae, the 3-10 water doubly of medical material weight will be added after Six-element Chinese crude drug co-grinding, soak 1-3 hour;
(2) the wet medical material obtained in step (1) is loaded in extraction vessel together with its soak, extract, obtain extracting solution;
(3) add natural clarifying agent in the merge extractive liquid, obtained to step (2), stir, temperature remains on 25-85 DEG C, and leave standstill after 1-8 hour, high speed centrifugation, gets supernatant;
(4) supernatant obtained in step (3) is carried out microporous filter, get Sang Jiang filtrate;
(5) the Mulberry Rhizoma Zingiberis Recens filtrate obtained in concentration step (4), get Sang Jiang extractum.
4. according to the Mulberry Rhizoma Zingiberis Recens leaching ointment preparation described in Claims 2 or 3, it is characterized in that: add 1-4 times of volume 60-90% ethanol after described step (3) and leave standstill 5-24 hour precipitation further, get supernatant.
5. according to the preparation method described in claim 4, it is characterized in that: the supernatant obtained after adding alcohol settling after described step (3) continues to add 1-3 times of volume distilled water and staticly settles further, obtains supernatant.
6. according to the preparation method described in Claims 2 or 3, it is characterized in that: extract in described step (2), extraction time is 1-4 time, further decocting extraction time is 2-8 hour.
7. according to the preparation method described in Claims 2 or 3, it is characterized in that: the natural clarifying agent in described step (3), for a kind of in chitosan, fruit juice 101 or ZTC1+1 II type, the preferably natural clarifying agent of ZTC1+1 II type.
8. according to the preparation method described in Claims 2 or 3, it is characterized in that: the natural clarifying agent in described step (3), for ZTC1+1 II type natural clarifying agent, 2%-10% and 4%-20% that the addition sequence of its composition A, B component is A after first B, further A, B component addition is respectively medicine liquid volume.
9. according to the preparation method described in claim 2, it is characterized in that: in described step (4), the aperture of micropore filtering film is 1.2 μm.
10. the preparation method according to claim 1-8, is characterized in that: described Mulberry Rhizoma Zingiberis Recens extractum, can according to need of production, the adjuvant being equipped with proper proportion makes Mulberry Rhizoma Zingiberis Recens tablet by corresponding technical process, Mulberry Rhizoma Zingiberis Recens capsule, Mulberry Rhizoma Zingiberis Recens granule, the preparations such as Mulberry Rhizoma Zingiberis Recens oral liquid, Mulberry Rhizoma Zingiberis Recens injection.
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