CN1456233A - Preparation of six component rehmannia root capsules - Google Patents

Preparation of six component rehmannia root capsules Download PDF

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CN1456233A
CN1456233A CN 03118618 CN03118618A CN1456233A CN 1456233 A CN1456233 A CN 1456233A CN 03118618 CN03118618 CN 03118618 CN 03118618 A CN03118618 A CN 03118618A CN 1456233 A CN1456233 A CN 1456233A
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毛友昌
毛晓敏
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Abstract

A process for preparing Chinese-medicine "Capsule of six components including rehmannia" including such steps as distilling tree peony bark to extract peonol, merging the distilling liquid with the decoction of rehmannia root, yam and alismatis rhizome, vacuum concentrating, depositing in alcohol, mixing with the alcohol reflux liquid of dogwood fruit, removing alcohol, mixing said peonol with cyclodextrin, extracting from tuckahoe and concentrating, mixing all together, and loading in capsules. Its advantages are high curative effect and quality.

Description

The preparation method of LIUWEIDIHUANG JIAONANG
Technical field
This invention relates to the processing technology technical field of Chinese patent medicine capsule, relates in particular to the preparation method of LIUWEIDIHUANG JIAONANG.
Background technology
Capsule is a kind of form of Chinese drug commonly used, according to the relevant drug act of China, production technology has great change to need as a kind of new drug research, former dosage form has six drugs containing rehmanniae soft capsule (recording in the 20 of Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation "), LIUWEIDIHUANG JIAONANG (recording) in the 8th of Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation ", six drugs containing rehmanniae sheet (recording) in the 8th of Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation ", the six drugs containing rehmanniae granule (records in become a full member the 9th of standard of new drug, the version Chinese Pharmacopoeia was one one in 2000), the six drugs containing rehmanniae oral liquid (records in become a full member the 14 of standard of new drug, 11), LIUWEI DIHUANG WAN (various honeyed pill) (record in 2000 version Chinese Pharmacopoeia one one), six drugs containing rehmanniae concentrated pill (recording) in one one of version Chinese Pharmacopoeia in 2000, the 11 in Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation.Honeyed pill, water-honeyed pill are that the full powder of medical material adds honey, and mulse is mixed to be made, and is characterized in having kept whole compositions, but difficult clothes.Concentrated pill is that Cortex Moutan extracts paeonol earlier, and residue and part Fructus Corni, Radix Rehmanniae Preparata, Rhizoma Alismatis decoct with water and be condensed into thick paste, and Rhizoma Dioscoreae beats fine powder with the residue Fructus Corni; With above thick paste, fine powder, paeonol mixing, pill, drying forms.Though dose reduces to some extent than honeyed pill, water-honeyed pill, dose still is on the high side, indissolubleization, and paeonol has loss in dry run.Tablet, capsule, granule are that three flavor medicated powder such as Cortex Moutan are broken into fine powder, and three flavors such as all the other Radix Rehmanniae Preparata are made the water thick paste, or add dextrin, correctives is made granule and formed granule, and is or mixed dry, pulverizes encapsulated forming, or be pressed into tablet.Though improve to some extent than honeyed pill, concentrated pill, dose is still bigger than normal, will obey 8 large capsules or 8 at every turn and is difficult to accept.Granule adds mixing in water for oral taking, and is also more convenient, but there are the shortcoming of the loss of volatile ingredient jointly in dry link in the technical process and tablet, capsule.Oral liquid be medical material through the decocting in water precipitate with ethanol, add correctives again, fill forms, though solved the problem of difficult clothes, for keeping clarity, in the precipitate with ethanol process, has lost many effective ingredient, thereby has influenced curative effect.Soft capsule is a kind of novel form, is characterized in the technology, according to the contained active component character design of different medical materials extraction process, and extract is significantly reduced, thereby makes soft capsule with the vegetable oil mixing.In pelletizing process, do not need through high temperature heating, reduced the loss of volatility, thermal sensitivity composition, thereby kept the curative effect of former pill.And need take 3 soft capsules, the patient is taken like a shot for each.But system soft capsule technical process is complicated, and specification requirement is higher, and production cost is higher relatively, and soft capsule content is oil extractum, disperses slower under one's belt.Based on above situation, the extraction process of soft capsule is applied in the capsule manufacturing, thereby obtain the little new LIUWEIDIHUANG JIAONANG of a kind of dose, overcome the weak point of all multi-pharmaceuticss, become a kind of convenient for productionly, reduced the loss of thermal sensitivity composition and volatile ingredient in the prescription again, guarantee curative effect and carry, a kind of new LIUWEIDIHUANG JIAONANG of taking convenience, society is given in contribution, benefits the common people.
Summary of the invention
The purpose of this invention is to provide the new preparation method of a kind of LIUWEIDIHUANG JIAONANG, improve the quality of products and curative effect, increase the stability of product, and dosage is little, produces, take, easy to carry, satisfy needs of medical treatment better.
The objective of the invention is such realization:
The preparation method of LIUWEIDIHUANG JIAONANG comprises the steps:
One, the prescription of LIUWEIDIHUANG JIAONANG is formed
Radix Rehmanniae Preparata 352-704g Cortex Moutan 132-264g Rhizoma Dioscoreae 176-352g
Fructus Corni 176-352g Rhizoma Alismatis 132-264g Poria 132-264g
Right amount of auxiliary materials is made 1000 altogether.
Its optimum formula is:
Radix Rehmanniae Preparata 470g Cortex Moutan 176g Rhizoma Dioscoreae 235g
Fructus Corni 235g Rhizoma Alismatis 176g Poria 176g
Right amount of auxiliary materials is made 1000 altogether.
Two, LIUWEIDIHUANG JIAONANG preparation technology
Technology one cleans the Six-element medicine respectively, removes impurity, and it is standby to be up to the standards; Become coarse powder standby Six-element medicine pulverize separately; Get Cortex Moutan and add water distillation, extract paeonol, adding cyclodextrin, to make the paeonol cyclodextrin clathrate standby; Water boiling liquid after distillation device is in addition collected; Fructus Corni is with 70% alcohol reflux secondary, and each 2 hours, merge extractive liquid, filtered filtrate for later use.Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, and being evaporated to relative density is the clear paste of 1.15-1.20 (50 ℃), put cold, add ethanol and make and contain alcohol amount and reach 70%, left standstill 48 hours, get the merging of supernatant and above-mentioned Fructus Corni extracting solution, decompression recycling ethanol is to there not being the alcohol flavor, and is standby; After Poria adds water boil, in 80 ℃ of warm macerating secondaries, each 1.5 hours, merge leachate, filter, being concentrated into relative density is the clear paste of 1.15-1.20 (50 ℃), merge with above-mentioned reserve liquid, being concentrated into relative density is the thick paste of 1.30 (50 ℃), and drying under reduced pressure is pulverized, add paeonol cyclodextrin clathrate and appropriate amount of auxiliary materials, mixing, encapsulated, promptly.
Technology two cleans the Six-element medicine respectively, removes impurity, and it is standby to be up to the standards; Become coarse powder standby Six-element medicine pulverize separately; Get Cortex Moutan and add water distillation, extract paeonol, adding cyclodextrin, to make the paeonol cyclodextrin clathrate standby; Aqueous solution after distillation device is in addition collected; Fructus Corni is with 70% alcohol reflux secondary, and each 2 hours, merge extractive liquid, filtered filtrate for later use.Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, and being concentrated into relative density is the clear paste of 1.15-1.20 (50 ℃), put cold, add ethanol and make and contain alcohol amount and reach 70%, left standstill 48 hours, get the merging of supernatant and above-mentioned Fructus Corni extracting solution, decompression recycling ethanol is to there not being the alcohol flavor, and is standby; After Poria adds water boil, in 80 ℃ of warm macerating secondaries, each 1.5 hours, merge leachate, filter, being concentrated into relative density is the concentrated solution of 1.05-1.15 (50 ℃), merge with above-mentioned reserve liquid, being concentrated into relative density is the concentrated solution of 1.05-1.15 (50 ℃), and spray drying is pulverized, add paeonol cyclodextrin clathrate and appropriate amount of auxiliary materials, mixing, encapsulated, promptly.
Three, prepared by technology one, two is capsule.
Added adjuvant can be in the technology: any or multiple mixing in micropowder silica gel, starch, dextrin, the magnesium stearate is used.
Powder of Fructus Corni is broken into coarse powder and was generally 10-40 purpose coarse powder in the technology, is preferably 30 order coarse powder.
Five tastes medical material such as all the other Radix Rehmanniae Preparata is ground into coarse powder and was generally 5-20 purpose coarse powder in the technology, is preferably 10 order coarse powder.
The condition of cornusol reflux, extract, secondary is in the technology: the each consumption of 60-90% ethanol is that the 5-10 of dose doubly measures, each 1-4 hour; Being preferably the each consumption of 70% ethanol is 6.5 times of amounts of dose, each 2 hours.
The condition that Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis decocting boil in the technology is: amount of water is doubly measured for the 4-10 of dose for the second time for doubly measuring for the 6-12 of dose for the first time, and the time is 2-6 hour for the first time, is 1-3 hour for the second time.The best is: amount of water is 10 times of amounts of dose for the first time, is 8 times of amounts of dose for the second time, and the time, second was 1 hour in order to be 2 hours for the first time.
The condition that the Poria decocting boils in the technology is: after the 4-10 times of water gaging that adds dose boils, and 70-90 ℃ of warm macerating secondary, each 1-3 hour; After 6 times of water gagings that are preferably dose boil, 80 ℃ of warm macerating secondaries, each 1.5 hours.
The relative density that is condensed into clear paste in the technology is 1.10-1.25 (50 ℃), and best relative density is 1.15-1.20 (50 ℃).
The relative density that is condensed into thick paste in the technology is 1.20-1.35 (50 ℃), and best relative density is 1.28-1.30 (50 ℃).
The relative density that is condensed into concentrated solution in the technology is 1.05-1.15 (50 ℃), and best relative density is 1.08-1.10 (50 ℃).
The condition of Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis clear paste precipitate with ethanol is in the technology: add alcohol and make and contain alcohol amount and reach 60-80%, leave standstill after 24-56 hour and get supernatant; Be preferably and add alcohol and make and contain alcohol amount and reach 70%, leave standstill after 48 hours and get supernatant.
The method for concentration of the decocting in water alcohol deposit fluid of water decoction, Poria water-leach liquor and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis in the technology: should adopt concentrating under reduced pressure/thin film concentration.
The method of Cortex Moutan water distillation and extraction paeonol is in the technology: Cortex Moutan is ground into coarse powder, the 15-25 times of water gaging that adds dose, soaked 1-3 hour, vapor distillation, the 8-15 that collects dose doubly measures distillate, the crystallization of leaching paeonol, filtrate adds sodium chloride to the 3-8% redistillation, and the 2-5 that collects dose doubly measures distillate, the crystallization of leaching paeonol, merge secondary crystallization, standby with cyclodextrin inclusion compound.Optimised process is: Cortex Moutan is ground into coarse powder, 20 times of water gagings that add dose, soaked 2 hours, vapor distillation is collected 10 times of dose and is measured distillates, the crystallization of leaching paeonol, filtrate adds sodium chloride to 5% redistillation, collects 3 times of amount distillates of dose, the crystallization of leaching paeonol, merge secondary crystallization, standby with cyclodextrin inclusion compound.
The spray drying inlet temperature is 100-200 ℃ in the technology, and leaving air temp is 50-150 ℃, and best inlet temperature is 160 ℃, and leaving air temp is 100 ℃.
Paeonol cyclodextrin clathrate preparation in the technology: cyclodextrin can adopt any in beta-schardinger dextrin-, the hydroxyl beta-schardinger dextrin-, the ratio of volatile oil and beta-schardinger dextrin-is 1: 5-15 (ml/g), optimal proportion is 1: 8 (ml/g), the ratio of volatile oil and hydroxyl beta-schardinger dextrin-is 1: 3-10 (ml/g), optimal proportion are 1: 5.5 (ml/g).
This invention and its superiority of original capsule manufacturing technology comparison are: production technology more becomes fully rationally, has overcome the loss of volatility active component and thermal sensitivity composition in the technology of former dosage form, also overcome dose and be difficult to the shortcoming accepted greatly, and quality standard has new raising again, makes the quality of product that guarantee arranged.
The specific embodiment
The optimum implementation of this invention is that the Six-element medicine is cleaned respectively, removes impurity, and it is standby to be up to the standards; Become coarse powder standby Six-element medicine pulverize separately; Get Cortex Moutan and add water distillation, extract paeonol, adding cyclodextrin, to make the paeonol cyclodextrin clathrate standby; Aqueous solution after distillation device is in addition collected; Fructus Corni is with 70% alcohol reflux secondary, and each 2 hours, merge extractive liquid, filtered filtrate for later use.Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, and being concentrated into relative density is the clear paste of 1.15-1.20 (50 ℃), put cold, add ethanol and make and contain alcohol amount and reach 70%, left standstill 48 hours, get the merging of supernatant and above-mentioned Fructus Corni extracting solution, decompression recycling ethanol is to there not being the alcohol flavor, and is standby; After Poria adds water boil, in 80 ℃ of warm macerating secondaries, each 1.5 hours, merge leachate, filter, being concentrated into relative density is the concentrated solution of 1.05-1.15 (50 ℃), merge with above-mentioned reserve liquid, being concentrated into relative density is the concentrated solution of 1.05-1.15 (50 ℃), and spray drying is pulverized, add paeonol cyclodextrin clathrate and appropriate amount of auxiliary materials, mixing, encapsulated, promptly.

Claims (1)

1. the preparation method of LIUWEIDIHUANG JIAONANG is characterized in that it may further comprise the steps:
(1) powder of Fructus Corni is broken into coarse powder and was generally 10-40 purpose coarse powder in the technology, is preferably 30 order coarse powder.
(2) Radix Rehmanniae Preparata, Cortex Moutan, Rhizoma Dioscoreae, Rhizoma Alismatis, Poria five tastes medical material pulverize separately became 5-20 purpose coarse powder in the technology, and it is standby to be preferably 10 order coarse powder.
(3) condition of cornusol reflux, extract, secondary is in the technology: the each consumption of 60-90% ethanol is that the 5-10 of dose doubly measures, each 1-4 hour; Being preferably the each consumption of 70% ethanol is 6.5 times of amounts of dose, each 2 hours.
(4) condition that Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis decocting boil in the technology is: amount of water is doubly measured for the 4-10 of dose for the second time for doubly measuring for the 6-12 of dose for the first time, and the time is 2-6 hour for the first time, is 1-3 hour for the second time.The best is: amount of water is 10 times of amounts of dose for the first time, is 8 times of amounts of dose for the second time, and the time, second was 1 hour in order to be 2 hours for the first time.
(5) condition that the Poria decocting boils in the technology is: after the 4-10 times of water gaging that adds dose boils, and 70-90 ℃ of warm macerating secondary, each 1-3 hour; After 6 times of water gagings that are preferably dose boil, 80 ℃ of warm macerating secondaries, each 1.5 hours.
(6) relative density that is condensed into clear paste in the technology is 1.10-1.25 (50 ℃), and best relative density is 1.15-1.20 (50 ℃); The relative density that is condensed into thick paste in the technology is 1.20-1.35 (50 ℃), and best relative density is that the relative density that is condensed into concentrated solution in 1.28-1.30 (50 ℃)/technology is 1.05-1.15 (50 ℃), and best relative density is 1.08-1.10 (50 ℃).The spray drying inlet temperature is 100-200 ℃, and leaving air temp is 50-150 ℃, and best inlet temperature is 160 ℃, and leaving air temp is 100 ℃.
(7) condition of Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis clear paste precipitate with ethanol is in the technology: add alcohol and make and contain alcohol amount and reach 60-80%, leave standstill after 24-56 hour and get supernatant; Be preferably and add alcohol and make and contain alcohol amount and reach 70%, leave standstill after 48 hours and get supernatant.
(8) method for concentration of the decocting in water alcohol deposit fluid of water decoction, Poria water-leach liquor and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis in the technology: should adopt concentrating under reduced pressure/thin film concentration.
(9) method of Cortex Moutan water distillation and extraction paeonol is in the technology: Cortex Moutan is ground into coarse powder, the 15-25 times of water gaging that adds dose, soaked 1-3 hour, vapor distillation, the 8-15 that collects dose doubly measures distillate, the crystallization of leaching paeonol, filtrate adds sodium chloride to the 3-8% redistillation, and the 2-5 that collects dose doubly measures distillate, the crystallization of leaching paeonol, merge secondary crystallization, standby with cyclodextrin inclusion compound.Optimised process is: Cortex Moutan is ground into coarse powder, 20 times of water gagings that add dose, soaked 2 hours, vapor distillation is collected 10 times of dose and is measured distillates, the crystallization of leaching paeonol, filtrate adds sodium chloride to 5% redistillation, collects 3 times of amount distillates of dose, the crystallization of leaching paeonol, merge secondary crystallization, standby with cyclodextrin inclusion compound.
(10) paeonol cyclodextrin clathrate preparation in the technology: cyclodextrin can adopt any in beta-schardinger dextrin-, the hydroxyl beta-schardinger dextrin-, the ratio of volatile oil and beta-schardinger dextrin-is 1: 5-15 (ml/g), optimal proportion is 1: 8 (ml/g), the ratio of volatile oil and hydroxyl beta-schardinger dextrin-is 1: 3-10 (ml/g), optimal proportion are 1: 5.5 (ml/g).
(11) (1), (2), (3), (4), (5), (6), (7), (8), (9), (10) are fed intake by national standard prescription consumption, mix, incapsulate, make LIUWEIDIHUANG JIAONANG.
CN 03118618 2003-02-12 2003-02-12 Preparation of six component rehmannia root capsules Pending CN1456233A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104000994A (en) * 2014-06-06 2014-08-27 余中华 Preparation method of concentrated six-taste glutinous rehmannia capsule

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104000994A (en) * 2014-06-06 2014-08-27 余中华 Preparation method of concentrated six-taste glutinous rehmannia capsule

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