CN101385750B - Preparation method of effective ingredient of isatis root - Google Patents
Preparation method of effective ingredient of isatis root Download PDFInfo
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- CN101385750B CN101385750B CN2007100500163A CN200710050016A CN101385750B CN 101385750 B CN101385750 B CN 101385750B CN 2007100500163 A CN2007100500163 A CN 2007100500163A CN 200710050016 A CN200710050016 A CN 200710050016A CN 101385750 B CN101385750 B CN 101385750B
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Abstract
The invention discloses a method for preparing active ingredients of radix isatidis, including steps of filtering, cleaning, drying, pulverizing, stage-one extracting, stage-one centrifugating, stage-two extracting, stage-one fractionating, stage-two centrifugating, stage-three extracting, stage-two fractionating and precipitating radix isatidis, thereby obtaining a finished active ingredients of radix isatidis. The method has the advantages of high yield, high output, energy saving, short production period and full automatic control. The prepared product has the functions of antibiosis, antivirus, antiendotoxin, anti-inflammation and immunity strengthening, and can be made into liquid injection, tablet, pill, powder, capsule, oral solution, etc.
Description
Technical field
The present invention relates to a kind of preparation method of Chinese herbal medicine extract, the preparation method more specifically to effective ingredient of isatis root belongs to the field of Chinese medicines.
Background technology
Radix Isatidis is the root of cruciferae isatis, has the effect of heat-clearing and toxic substances removing, removing heat from blood.Contain in the Radix Isatidis extract that many sinigrins, indirubin, indigo are beautiful blue, indigo-blue, compositions such as earthworm diindyl glycoside, BETA-sitosterol, adenosine, Palmic acid and several amino acids, have characteristics such as antibiotic, antiviral, antiendotoxin, antiinflammatory, raise immunity.The palette backboard is the same with other Chinese herbal medicine, and composition is very complicated, and existing effective ingredient has invalid components and toxic component again.In order to improve the therapeutic effect of Chinese herbal medicine such as Radix Isatidis, will use up effective component extracting to greatest extent, remove invalid components and toxic component.Therefore, the extraction of Radix Isatidis is the most important for the inherent quality and the clinical efficacy that improve Chinese medicine preparation.
Chinese herbal medicine extracting method commonly used has decocting method, hydrodistillation, circumfluence method, infusion process, percolation etc., and these its advantages of traditional extraction process are easy and simple to handle, is not very high to the requirement of technology, equipment, uses comparatively extensive.But much more very shortcomings are also arranged, decoct the temperature height as all existing usually, the time is long, big problem consumes energy; Keeping effective ingredient, remove the invalid components aspect, exist the problem that loss of effective components is big, the cycle long, operation is many, extraction ratio is not high; Contain more impurity in the extracting solution simultaneously,, thereby influence the effective ingredient extraction rate to next step refining making troubles; Decoction and alcohol sedimentation technique commonly used comes impurity removal and purification because in a large number with an organic solvent, poor stability, reclaim loaded down with trivial details, cost height, and serious environment pollution.The former process using decocting method and the ethanol precipitation of preparation effective ingredient of isatis root are produced, exist and decoct temperature height, time length, big, the many shortcomings such as loss of effective components is big, operation is many, extraction ratio is low, contaminated environment of power consumption, and product percent of pass is extremely low, cause the product cost height, influenced economic benefit of enterprises.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts chloroform dynamic extraction technology to extract effective ingredient of isatis root, use this method can make the active ingredient recovery rate height of Baphicacanthus cusia plate, the output height, and also this method can energy savings, with short production cycle, can Automatic Control.
The invention provides the preparation method of a kind of Baphicacanthus cusia plate active ingredient, this method comprises the step of following order:
(1) screening: Radix Isatidis is chosen debug eat into go mouldy product and impurity, sieve removes silt, chooses medicinal part and removes the non-medicine part position;
(2) clean: will screen back Radix Isatidis medical material and drop into clear water, and eluriate the back and in time take out;
(3) oven dry: the Radix Isatidis medical material after the cleaning is in time dried, and temperature is controlled at 50-80 ℃, and moisture content reaches below 10%;
(4) pulverize: the Radix Isatidis pulverizing medicinal materials of oven dry is become coarse powder, cross 20 mesh sieves;
(5) one-level extraction: the Radix Isatidis coarse powder after the pulverizing, carry out continuous countercurrent extraction by placed in-line three grades of decanters with 5-8 chloroform extraction liquid doubly;
(6) first-stage centrifugal: the liquid after the one-level extraction adds 101 clarifiers, and earlier through the centrifugal extractor centrifugal clarification, rotating speed is 2500-4000r/min;
(7) secondary extraction: the effective ingredient after the first-stage centrifugal clarification contacts with the acidifying water of PH5-7, and in solvent phase, solvent phase obtains Radix Isatidis extract stock solution and chloroform extraction liquid through concentrating through three grades of placed in-line centrifugal extractor back extractions;
(8) one-level rectification: the chloroform extraction liquid after the secondary extraction is through distillation column rectification, and the chloroform extraction solvent enters the circulation of one-level extraction process after fractional distillation, and pressure is 2-5Mpa, and temperature is 35 ℃;
(9) secondary is centrifugal: the Radix Isatidis extract stock solution after the secondary extraction is through the centrifugal impurity of removing of centrifuge, and rotating speed is 3500-4500r/min;
(10) three grades of extractions: the effective ingredient after secondary is centrifugal contacts with the acidifying water of PH5-7, and again through three grades of placed in-line extractor purification, solvent phase obtains Radix Isatidis extract concentrated solution and chloroform extraction liquid through concentrating;
(11) two-stage rectification: the chloroform extraction liquid after three grades of extractions fractionates out the chloroform extraction solvent and enters three grades of extraction process circulations after distillation column rectification, and pressure is 2-5Mpa, and temperature is 35 ℃;
(12) precipitation: extract makes finished product through post precipitation.
Described acidifying water is to mix with hydrochloric acid or sulphuric acid and water.
Because the present invention adopts the technology of above-mentioned dynamic extraction, its characteristics just are to increase under the situation of medical material specific surface area more than 200 times, utilize mechanical means such as filter press, forced circulation is to strengthen the solid-liquid contact, and simultaneously, it is poor to remain relative concentration between Radix Isatidis and the solvent, thereby realizes biphase continuous countercurrent operation, therefore the dissolution efficiency of the solute in the medical material to solvent has been improved more than 30 times.With respect to the Chinese medicine extraction process, dynamic extraction can make extract quality be greatly improved, and the extract active constituent content the highest 32% brings up to present 75% when adopting old technology; The product recovery rate obviously improves, and 43% brings up to present 89% when in the past high; Energy savings is extracted temperature and is reduced to present 40 ℃ by in the past the highest near 100 ℃, thereby saved a large amount of energy, and cuts down the consumption of energy 62%; Help to improve working environment, adopt new technology and also reduced the danger in working strength of workers and when operation significantly; In addition, can realize serialization production after adopting dynamic extraction technology, be convenient to Automatic Control, thereby can improve raw material, the energy and usage ratio of equipment, increase output, shortened the production cycle, need week age to be reduced to the present time by a collection of product of former production, thereby and reduce artificial error by reducing production link, reduce defective work, reduce cost, this product reduces by 53% because of resulting cost after changing each key element of production technology at present, and meet domestic and international Chinese medicine and do not have alcohol extraction, the environmental requirement of energy-saving and emission-reduction obtains extremely good social benefit and economic benefit in a short time.
The present invention also is applicable to the preparation as Chinese herbal medicine effective ingredientses such as Herba Andrographis.
Description of drawings
Fig. 1 is a technological process block-diagram of the present invention;
The specific embodiment
Further set forth the preparation method of medicine of the present invention below according to embodiment.
Embodiment 1
By shown in Figure 1, a kind of preparation method of effective ingredient of isatis root comprises the steps:
(1) screening: Radix Isatidis is chosen debug eat into go mouldy product and impurity, sieve removes silt, chooses medicinal part and removes the non-medicine part position;
(2) clean: will screen back Radix Isatidis medical material and drop into clear water, and eluriate the back and in time take out;
(3) oven dry: the Radix Isatidis medical material after the cleaning is in time dried, and temperature is controlled at 70 ℃, and moisture content reaches below 8%;
(4) pulverize: the Radix Isatidis pulverizing medicinal materials of oven dry is become coarse powder, cross 20 mesh sieves;
(5) one-level extraction: the Radix Isatidis coarse powder 100Kg after the pulverizing, carry out continuous countercurrent extraction by placed in-line three grades of decanters with chloroform extraction liquid 520L;
(6) first-stage centrifugal: the liquid after the one-level extraction adds 101 clarifier 1500ml, and earlier through the centrifugal extractor centrifugal clarification, rotating speed is 3500r/min;
(7) secondary extraction: the effective ingredient after the first-stage centrifugal clarification is that 5.5 acidifying waters contact with 100L, PH, through three grades of placed in-line centrifugal extractor back extractions in solvent phase; Solvent phase obtains Radix Isatidis extract stock solution 75L and chloroform extraction liquid through concentrating;
(8) one-level rectification: the chloroform extraction liquid after the secondary extraction is through distillation column rectification, and the chloroform extraction solvent enters the circulation of one-level extraction process after fractional distillation, and pressure is 3Mpa, and temperature is 35 ℃;
(9) secondary is centrifugal: the Radix Isatidis extract stock solution after the secondary extraction is through the centrifugal impurity of removing of centrifuge, and rotating speed is 3500r/min;
(10) three grades of extractions: the effective ingredient after secondary is centrifugal is that 5.5 acidifying waters contact with 100L, PH, again through three grades of placed in-line extractor purification; Solvent phase obtains Radix Isatidis extract concentrated solution 45L and chloroform extraction liquid through concentrating;
(11) two-stage rectification: the chloroform extraction liquid after three grades of extractions fractionates out the chloroform extraction solvent and enters three grades of extraction process circulations after distillation column rectification, and pressure is 3Mpa, and temperature is 35 ℃;
(12) precipitation: extract makes the 45L finished product through post precipitation.
Claims (2)
1. the preparation method of an effective ingredient of isatis root, this method comprises the step of following order:
(1) screening: Radix Isatidis is chosen debug eat into go mouldy product and impurity, sieve removes silt, chooses medicinal part and removes the non-medicine part position;
(2) clean: will screen back Radix Isatidis medical material and drop into clear water, and eluriate the back and in time take out;
(3) oven dry: the Radix Isatidis medical material after the cleaning is in time dried, and temperature is controlled at 50-80 ℃, and moisture content reaches below 10%;
(4) pulverize: the Radix Isatidis pulverizing medicinal materials of oven dry is become coarse powder, cross 20 mesh sieves;
(5) one-level extraction: the Radix Isatidis coarse powder after the pulverizing, carry out continuous countercurrent extraction by placed in-line three grades of decanters with 5-8 chloroform extraction liquid doubly;
(6) first-stage centrifugal: the liquid after the one-level extraction adds 101 clarifiers, and earlier through the centrifugal extractor centrifugal clarification, rotating speed is 2500-4000r/min;
(7) secondary extraction: the effective ingredient after the first-stage centrifugal clarification contacts with the acidifying water of pH5-7, and in solvent phase, solvent phase obtains Radix Isatidis extract stock solution and chloroform extraction liquid through concentrating through three grades of placed in-line centrifugal extractor back extractions;
(8) one-level rectification: the chloroform extraction liquid after the secondary extraction is through distillation column rectification, and the chloroform extraction solvent enters the circulation of one-level extraction process after fractional distillation, and pressure is 2-5Mpa, and temperature is 35 ℃;
(9) secondary is centrifugal: the Radix Isatidis extract stock solution after the secondary extraction is through the centrifugal impurity of removing of centrifuge, and rotating speed is 3500-4500r/min;
(10) three grades of extractions: the effective ingredient after secondary is centrifugal contacts with the acidifying water of pH5-7, and again through three grades of placed in-line extractor purification, solvent phase obtains Radix Isatidis extract concentrated solution and chloroform extraction liquid through concentrating;
(11) two-stage rectification: the chloroform extraction liquid after three grades of extractions fractionates out the chloroform extraction solvent and enters three grades of extraction process circulations after distillation column rectification, and pressure is 2-5Mpa, and temperature is 35 ℃;
(12) precipitation: extract makes finished product through post precipitation.
2. effective ingredient of isatis root preparation method according to claim 1 is characterized in that: described acidifying water is to mix with hydrochloric acid or sulphuric acid and water.
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| CN101385750B true CN101385750B (en) | 2011-09-28 |
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| CN102670688A (en) * | 2012-05-22 | 2012-09-19 | 广西天天乐药业股份有限公司 | Active ingredient extract of isatis roots and preparation method for active ingredient extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1520837A (en) * | 2003-01-30 | 2004-08-18 | 普文英 | Plant extract and compound for treating endotoxin blood disease, and its extraction method and application |
| CN1544067A (en) * | 2003-11-26 | 2004-11-10 | 张晴龙 | Effervescence tablet of radix isatidis and its preparation |
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| CN1520837A (en) * | 2003-01-30 | 2004-08-18 | 普文英 | Plant extract and compound for treating endotoxin blood disease, and its extraction method and application |
| CN1544067A (en) * | 2003-11-26 | 2004-11-10 | 张晴龙 | Effervescence tablet of radix isatidis and its preparation |
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Owner name: SICHUAN PROVINCE TAIXINANIMAL PHARMACEUTICAL CO., Free format text: FORMER OWNER: SICHUAN KEWANG BIOTECHNOLOGY CO., LTD. Effective date: 20090515 |
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Effective date of registration: 20090515 Address after: North Economic Development Zone Xiang Yao Wan Village in Sichuan city of Suining Province Applicant after: Sichuan Taixin Animal Pharmaceutical Co., Ltd. Address before: No. 500 Mingyue Road, Suining Economic Development Zone, Sichuan Applicant before: Sichuan Kewang Biotechnology Co., Ltd. |
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