CN103393780B - Extraction method of high-purity coptis total alkaloid - Google Patents
Extraction method of high-purity coptis total alkaloid Download PDFInfo
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Abstract
The invention relates to an extraction method of high-purity coptis total alkaloid, which comprises the following steps: preparing a raw material (coptis or coptis fibril or coptis ash), pulverizing (not required if the raw material is coptis fibril or coptis ash), immersing in 0.1-5% sulfuric acid, heating and extracting four times, filtering, neutralizing with calcium oxide (or calcium hydroxide), filtering, washing the precipitate, preconcentrating, regulating the acid, precipitating with sodium chloride, filtering, recovering alkaloid from the mother liquor, and drying the precipitate to obtain the coptis total alkaloid product. The main active components of the product are coptis effective components, such as berberine, coptisine, palmatine, epiberberine, jateorhizine and the like; the coptis total alkaloid content is more than 50%; and the berberine content is more than 25%. The product provided by the invention has favorable actions of lowering blood sugar and blood fat, losing weight and the like, and is an ideal raw material for treating diabetes and cardiovascular diseases.
Description
Technical field
The invention belongs to biological extraction technology, be specifically related to a kind of high purity Rhizoma Coptidis total alkaloids extractive technique.
Background technology
The coptis begins to be loaded in
shennong's Herbal, be classified as top grade.Coptis bitter, cold in nature, there is the function of purging intense heat, removing toxic substances, heat-clearing, eliminating dampness., vomiting full for dysphoria with smothery sensation coma, vexed insomnia, damp and hot ruffian, bellyache and diarrhea dysentery, hot eyes pyogenic infections, ulceration on the oral mucosa and the tongue, eczema, scald, haematemesis, bleeding from five sense organs or subcutaneous tissue etc.Modern pharmacy result of study shows, coptis main active ingredient is Rhizoma Coptidis total alkaloids, mainly comprises (" Chinese Pharmacopoeias " 2010 editions) such as Berberine (berberine), palmatine, coptisine, epiberberine and jateorhizines; The coptis (element) has reducing blood-fat and the pharmacologically active widely such as hypoglycemic.Nearest research finds, except berberine, coptis related alkaloids activeconstituents (coptisine, palmatine etc.) also has reducing blood-fat and hypoglycemic grade acts on (Hou Hong etc.Rhizoma Coptidis alkaloid anti-hyperlipidemia and atherosclerosis experimental study.Time precious traditional Chinese medical science traditional Chinese medicines, 2011,22(10): 2462.); Also find simultaneously, highly purified Rhizoma Coptidis alkaloid security is very high, and Rhizoma Coptidis alkaloid crude product will cause the safety issues (Jun Yi etc. Safety evaluation of main alkaloids from Rhizoma Coptidis. Journal of Ethnopharmacology, 2013.145:303-310) such as liver function rising.Therefore, extract highly purified Rhizoma Coptidis total alkaloids and there is good Development volue, and the Rhizoma Coptidis alkaloid of low-purity is worth very little.In addition, coptis price is very expensive, and the yield improving Rhizoma Coptidis total alkaloids is the key reducing production cost and improve overall economic efficiency.
At present, the extraction process technology about Rhizoma Coptidis total alkaloids has more bibliographical information.
Chinese patent literature (200510044345.8) reports a kind of Rhizoma Coptidis total alkaloids extractive technique, mainly comprises: Rhizoma Coptidis, and with soak by water, upper macroporous resin purification, washing, aqueous ethanol wash-out, reclaim ethanol, concentrate drying, obtains the processes such as product.Its Rhizoma Coptidis total alkaloids content reaches 25 ~ 100%.According to our research experience, the extraction yield of the total alkaloidss such as the coptis directly uses soak by water, berberine is poor; On Rhizoma Coptidis alkaloid after resin, during wash-out, resin is difficult to 100% regeneration, and resin rate of utilization is not high; When reclaiming ethanol, ethanol inevitably loses and high energy consumption etc., causes cost increase etc.
Chinese patent literature (
200810069671.8) report a kind of coptis chinensis total alkaloid extracting technique technology, mainly comprise: raw material (coptis or coptis fibrous root or Chinese goldthread leaf) and---pulverize (as do not needed to pulverize for coptis fibrous root or Chinese goldthread leaf)---the sulfuric acid adding appropriate 0.01 ~ 10% soaks---intensification extraction four times---pre-concentration---purification---sodium-chlor and high-valency metal salt precipitation---filtration---oven dry---Rhizoma Coptidis total alkaloids product.The main active ingredient of product is the coptis effective constituents such as berberine, coptisine, jateorhizine, palmatine, epiberberine, and Rhizoma Coptidis total alkaloids content is more than 20%, wherein the content more than 10% of berberine.The Rhizoma Coptidis total alkaloids content (25%) on the low side that this Technology is produced, Product Safety is not high; Also containing a large amount of alkaloids in mother liquor after extract total alkaloids, be not recovered utilization, alkaloid total recovery is not high; In order to improve the purity of Rhizoma Coptidis total alkaloids, need to utilize sorbent material (as atlapulgite, silica gel, gac or various macroporous resins etc.) to purify, and the operation such as recrystallization, technique is comparatively complicated, and production cost is high.
Chinese patent literature (02103880.5) reports extraction process and the novelty teabag thereof of Rhizoma Coptidis total alkaloids, mainly comprise: coptis water soaking and time ultrasonication, total alkaloids extraction is carried out under temperature leaching condition, gained extracting solution carries out concentrating under reduced pressure, then the pH value of concentrated extracting solution is regulated with concentrated hydrochloric acid, add sodium-chlor again, leave standstill, then the throw out in extracting solution is collected by suction filtration or centrifuge dripping, throw out is dried, throw out after oven dry is pulverized, and can obtain Rhizoma Coptidis total alkaloids hydrochloride finished product.This explained hereafter is not owing to having purification process, and the purity of total alkaloids is not high; Meanwhile, owing to not reclaiming the total alkaloids in mother liquor, the yield of total alkaloids is not high yet.
Chinese patent literature (200610024364.9) reports a kind of total alkaloids of meadowrueleaf corydalis root and purification process thereof and pharmaceutical composition, mainly comprise: filter after total alkaloids of meadowrueleaf corydalis root crude extract sour water is dissolved, filtrate passes through macroporous adsorptive resins, first carry out wash-out with water, then wash-out is carried out with the ethanol of 10-45%, collect the elutriant of ethanolic moiety, concentrated, be drying to obtain total alkaloids of meadowrueleaf corydalis root.This technique needs a large amount of ethanol elution purifying, and production cost is difficult to control.
Chinese patent literature (201110053453.7) reports a kind of method utilizing polyamide resin separation and purification Rhizoma Coptidis alkaloid, mainly comprise: coptis crude extract polymeric amide is upper polyamide column after mixing sample, with dichloromethane eluent or the mixed solvent gradient elution with methylene dichloride and methyl alcohol, with thin-layer chromatography inspection stream part, merge same stream part, drying, namely separablely obtains seven alkaloids such as Berberine, palmatine, coptisine, palmatine, jateorhizine, magnoflorine, Groenlandcine.What this Technology was separated is Rhizoma Coptidis alkaloid monomer, and owing to relating to the very large methylene dichloride equal solvent of toxicity in separation and purification process, security is difficult to ensure.
Chinese patent literature (200810218824.0) reports Total base coptis and is preparing the application in treating diabetic complications medicine, mainly comprises: 1) Rhizoma Coptidis is ground into meal; 2) 5-10 times amount 60-80% ethanol is by coptis meal refluxing extraction 1-3 time, 1-2h/ time, and gradation is filtered, merging filtrate.Concentrating under reduced pressure, dry, obtain Rhizoma Coptidis extract; 3) Rhizoma Coptidis extract is added 5 times amount 0.5% sulfuric acid dissolutions, filter, filtrate adjusts pH9 with milk of lime respectively, filters, adjusts pH1 ~ 2 respectively, add sodium-chlor and make saltiness reach 10%, shake up with hydrochloric acid, leaves standstill, obtains Total base coptis.This technique does not relate to the problems such as the recovery of Rhizoma Coptidis total alkaloids in the rear mother liquor of Rhizoma Coptidis total alkaloids precipitation yet.
Chinese patent literature (201110243033.5) reports the purposes of Rhizoma Coptidis total alkaloids effervescent tablet method for making and treatment disease in the female sexual system, mainly comprise: get coptis plant herb appropriate, be crushed to meal, adding 4 ~ 15 times amount concentration is the aqueous sulfuric acid of 0.1 ~ 1%, soak at room temperature extracts 24 hours, filters for 2 ~ 5 times; Get extracting solution and add milk of lime tune pH7, place 8 ~ 12 hours, filter; Get extracting solution and add concentrated hydrochloric acid tune pH2-3, place 8 ~ 12 hours, filter: get precipitation and add 50 times amount water boils dissolvings, pH8-9 adjusted by milk of lime, filtered while hot; Get filtrate washing, drain, dry, obtaining Rhizoma Coptidis total alkaloids is a; 2 ~ 5 parts of polyethylene glycol 6000s add 5 ~ 15 parts of dissolve with ethanol, add 15 ~ 30 parts of sodium bicarbonates, obtain sodium bicarbonate, polyoxyethylene glycol, alcohol mixeding liquid be b; Adopt the spray starch absorption dehydration method of minigel preparation method, by b in the revolving pan that atomizer sparges splendid attire a, finally cross No. two whole grains of sieve and become c; Citric acid is crossed No. two sieve into particle and c cross No. seven sieve together with mix, compressing tablet, the heavy 1g of every sheet, feeding port place infrared ray radiation during compressing tablet.This invention is easy to carry, rapid-action, treatment disease in the female sexual system effect and definite and high curative effect.After this technique does not relate to Rhizoma Coptidis total alkaloids precipitation yet, the problem such as recovery of Rhizoma Coptidis alkaloid in mother liquor.
Chinese patent literature (201010246367.3) reports the novelty teabag of coptis total alkaloid extract, mainly comprises: the preparation method of coptis total alkaloid extract; So-called Rhizoma Coptidis total alkaloids is concentrated into dry after referring to that the certain water gaging heating of Rhizoma Coptidis is extracted.The Rhizoma Coptidis total alkaloids that this technique obtains is actually the full medicinal extract of the coptis, and purity is very low.
Chinese patent literature (200710099687.9) reports total alkaloids of meadowrueleaf corydalis root and preparation method thereof and purposes, the production method of its total alkaloids is: after raw material adds the sulphuric acid extraction of 0.1 ~ 1%, extracting solution adds sodium-chlor precipitation and saltouts, obtain total alkaloids and be dissolved in ethanol again, decolouring purifying, obtains the total alkaloids that purity is higher.After this technique precipitation total alkaloids, do not consider the recovery of total alkaloids in mother liquor, affect final yield; Crude product is dissolved in ethanol, and decolouring purifying, will affect the yield of total alkaloids further.
" Rhizoma Coptidis alkaloid extracts and purifying process research " (Tu Yaosheng etc.New Chinese medicine and clinical pharmacology.2012,23(2): 208) report a kind of Rhizoma Coptidis total alkaloids and extract and purification process, mainly comprise: coptis medicine materical crude slice adds the sulphuric acid soln of 8 times amount 1.5 %, decoct 3 times, each 40 min; Rhizoma extracting liquid is with Ca (OH)
2regulate pH5 ~ 6, suction filtration, it is that every mL contains 0.24g crude drug, suction filtration that filtrate heating is concentrated into concentration, and filtrate salt adding acid for adjusting pH 1.5 ~ 2, adds 5% sodium chloride solution and make dissolving, hold over night in refrigerator, suction filtration, filter residue vacuum-drying (50 DEG C), collects purified.Rhizoma Coptidis total alkaloids extraction yield about 93%, total alkaloids yield about 60%, total alkaloids purity about 84%.This technique total alkaloids yield (60%), and the purity of product is also general.
In sum, although the Technology extracting Rhizoma Coptidis total alkaloids is very many, ubiquity total alkaloids yield is not high, or purity is undesirable, or complex process, or relates to the problems such as noxious solvent in the course of processing.
In the art, extraction yield refers to the biological alkali number be dissolved into from the coptis in solution, the product volume that yield finally obtains after being through extraction operation.But the amount be dissolved in solution is many, might not finally obtain many, because can there is various loss in subsequent processes, some losses can be very large.
And from the report of prior art, prior art does not all consider that in mother liquor, alkaloid recovery and precipitation take away alkaloidal recovery, mainly there is blind spot in research: namely many research workers did not carry out systems analysis, and do not know sealed Belt walks how many alkaloids, mother liquor takes away how many alkaloids, namely and do not know alkaloid which step have lost, thus do not want reclaim alkaloidal problem.
Summary of the invention
The object of the present invention is to provide a kind of high purity Rhizoma Coptidis total alkaloids extracting method, it for raw material with the coptis and by product thereof, namely extracts the total alkaloids in the coptis and coptis fibrous root and coptis lime-ash, improves purity and the yield of its finished product simultaneously.
The present invention is with the coptis and coptis plant for raw material, and adopt sulphuric acid soln soak extraction to produce Rhizoma Coptidis total alkaloids, described method comprises:
1), raw material prepares
The coptis or coptis fibrous root or coptis lime-ash are removed silt, pulverizes or chopping (as do not needed to pulverize or chopping for coptis fibrous root or coptis lime-ash), as the raw material processed.
2), soak
Raw material joined fermentation vat or extract in still, add appropriate (3 ~ 15 times of volumes) concentration be 0.1 ~ 5% aqueous sulfuric acid (W/V) soak 1 ~ 48 hour.
3), extract
After immersion, be warmed up to 20 ~ 100 DEG C, insulation extraction 0.1 ~ 5 hour, extracts four times.First time and second time extracting solution are for the production of product; Third time, extracting solution was used for the soak solution of next batch raw material, and soak solution is directly as primary extracting solution; No. the 4th extracting solution is used for the second time extracting solution of next batch raw material.
4), feed liquid neutralization
To merge with second time extracting solution first time, filter; Filtrate, with pH=2 ~ 12 of lime (or calcium hydroxide) neutralization to solution, is filtered; Residue uses in right amount (0.1 ~ 3 times of level of residue) water washing 1 ~ 3 time again, reclaims the alkaloid that residue is taken away.Washings stays, and merges, utilize macroporous resin treatment to the 8th step and total alkaloids mother liquor of precipitation of ammonium.
5), saltout
By pH=1 ~ 5 of neutralizer with concentrated hydrochloric acid regulator solution; Then, add the sodium-chlor of liquor capacity 1 ~ 20% ratio, low temperature (0 ~ 30 DEG C) is placed 1 ~ 48 hour, precipitation total alkaloids.
For the 4th) neutralizer after the filtration of step, also can carry out pre-concentration, namely carry out concentrating under reduced pressure 1 ~ 20 times, and then carry out the 5th step.
6), filter and wash
Precipitation (total alkaloids) adopts natural filtration or centrifuging, simultaneously with suitable quantity of water washing, is Rhizoma Coptidis total alkaloids.
7), total alkaloids mother liquid disposal
The washing lotion of the mother liquor after precipitation total alkaloids and the operation of the 4th step merges, according to macroporous resin in the speed of per minute 0.1 ~ 5% times of resin volume, after macroporous resin adsorption, with the water washing resin of 0.1 ~ 5 times of macroporous resin volume; Then the ethanol elution of 10 ~ 90%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids.
8), dry
Merge two steps and operate the Rhizoma Coptidis total alkaloids obtained, dry, be high purity Rhizoma Coptidis total alkaloids product.The main active ingredient of this product is the Rhizoma Coptidis total alkaloidss such as berberine (Berberine), coptisine, epiberberine, palmatine, jateorhizine.The yield more than 90% of total alkaloids, the content more than 50% of Rhizoma Coptidis total alkaloids, the wherein content more than 25% of berberine.
Under normal circumstances, in this product, total alkaloid content is generally about 90%, and berberine content can reach 45%, and other biological alkali content can reach 45%, is more than 9 times of total alkaloid content in the coptis.
Alkaloid yield of the present invention is high, the yield more than 90% of total alkaloids, simple to operate, and industrial cost is reduced greatly, and productivity effect significantly improves; The product purity that the present invention produces is high, and generally can reach more than 90%, security is fabulous; The Rhizoma Coptidis total alkaloids that the present invention obtains and composition thereof, very similar with the composition of Rhizoma Coptidis total alkaloids, there is pharmacological properties like Rhizoma Coptidis, have more preferably hypoglycemic, the effect such as reducing blood-fat and fat-reducing than the single coptis.
Product of the present invention (Rhizoma Coptidis total alkaloids) can, as the surrogate of the products such as the coptis, coptis concentrated product, berberine, may be used for treating diabetes, hyperlipidemia, obesity and cardiovascular disease.
below the Rhizoma Coptidis total alkaloids that obtains of relevant the present invention and common berberine security and the contrast experiment that treats in relative disease:
1., subchronic toxicity testing
Test materials is Rhizoma Coptidis total alkaloids (content 90%), berberine (content 95%), the Rhizoma Coptidis total alkaloids crude product (total alkaloid content 40%) that the present invention obtains.
Subchronic toxicity testing method is carried out with reference to " natural drug (Chinese medicine) new drug research governing principle ": SD rat is divided into four groups, be respectively Normal group, Rhizoma Coptidis total alkaloids group, berberine group, Rhizoma Coptidis total alkaloids crude product group, often organize 10, dosage is 1g/Kg; Continuous irrigation is fed 3 months, then adopts the biochemical indicators such as fasting blood monitoring liver function.
From table can see, compared with Normal group, Rhizoma Coptidis total alkaloids sterling on liver function without any impact; The liver of Berberine on laboratory animal does not also affect; The liver function of Rhizoma Coptidis total alkaloids crude product group mouse obviously raises, and shows that the liver of the Rhizoma Coptidis total alkaloids of low-purity to animal has disadvantageous effect.The result of this result and bibliographical information is similar (Jun Yi etc. Safety evaluation of main alkaloids from Rhizoma Coptidis. Journal of Ethnopharmacology, 2013.145:303-310).
2., hypolipidemic activity experiment
Test materials is Rhizoma Coptidis total alkaloids (total alkaloid content 90%), berberine (content 95%), the Rhizoma Coptidis total alkaloids crude product (total alkaloid content 40%) that the present invention obtains.
Lipid-lowering test method is carried out with reference to " natural drug (Chinese medicine) new drug research governing principle ": Golden Hamster is divided into 5 groups, one group (10) give chow diet, and one group (40) give high lipid food; After 4 weeks, detect blood lipids index, more successful for modeling Golden Hamster is divided into 4 groups (often organizing 8 ~ 10): high fat control group, Rhizoma Coptidis total alkaloids group, berberine group, Rhizoma Coptidis total alkaloids crude product group.Medicine group gives 500mg/Kg medicine; Continuous irrigation is fed 4 weeks, then adopts fasting blood and detects blood lipids index.
Can see from table, compared with Normal group, each test group blood fat all has rising, shows modeling success; Compared with high fat group, each medicine group cholesterol (TC) declines all to some extent, shows all have hypolipidemic activity; Wherein the hypolipidemic activity of high purity total alkaloids is better than Berberine, is also better than total alkaloids crude product.
Above-mentioned result of study shows, no matter from security or from drug effect aspect, highly purified Rhizoma Coptidis total alkaloids value of exploiting and utilizing is obviously better than the Rhizoma Coptidis total alkaloids of low-purity.
The present invention has the following advantages:
1., this Technology with the coptis and by product thereof for raw material, especially with by products such as coptis fibrous root and coptis lime-ash for raw material, belong to comprehensive utilization of resources scope, low cost product, the course of processing is simple, is easy to preparation.
2., in the product that obtains of this Technology except berberine, still containing a large amount of coptis related alkaloids such as palmatine, coptisine, epiberberine, jateorhizine, biological value is higher, and the utilization of resources is more abundant.
3., extracting solution by lime (or calcium hydroxide) neutralisation of sulphuric acid, utilize calcium sulfate to adsorb impurity in removing extracting solution, ensure that the quality of salt precipitation total alkaloids.Compared with other impurity and purification techniques, this technological operation is simple, with low cost.
4., utilize macroporous resin treatment Rhizoma Coptidis total alkaloids to precipitate after mother liquor and the washing lotion of calcium sulfate precipitation, not only reclaimed the total alkaloids that mother liquor and calcium sulfate precipitation are taken away, ensure that the yield of Rhizoma Coptidis total alkaloids; And by after macroporous resin adsorption, ion, significantly improves the purity of total alkaloids.The overall extraction yield more than 90% of this technique Rhizoma Coptidis total alkaloids, the content (purity) about 90% of total alkaloids.Simple to operate, practical.
5.,this technology utilization calcium sulfate precipitation adsorption-edulcoration, reclaims the most of Rhizoma Coptidis alkaloid (about 60%) extracted; Recycling macroporous resin adsorption reclaims the Rhizoma Coptidis alkaloid in mother liquor and precipitation, not only reduces cost, improves product purity, and ensure that total recovery.Technology is simple, and comparative costs is low.
Embodiment
embodiment 1:
1 kilogram of coptis is pulverized or section, adds the sulphuric acid soln of 3 liter 5%, soaks after 1 hour, be warmed up to 100 DEG C of refluxing extraction 0.1 hour, filter; Residue is warmed up to 100 DEG C of extractions three times with the sulphuric acid soln of 3 liter 5% again; Merging first time and the second extracting solution (extract for three times and extract the process being used for next batch raw material four times), separate supernatant liquor after cooling (or filtration obtains supernatant liquor); Supernatant liquor utilizes lime (calcium oxide) to neutralize pH=2, filters, and precipitation utilizes the water washing of 0.1 times of precipitation capacity to precipitate 3 times; Neutralizer utilizes about the pH=1 of concentrated hydrochloric acid regulator solution, and the sodium-chlor adding 1% fully stirs rear room temperature (30 DEG C) static 48 hours; Filter, precipitation suitable quantity of water washs three times, obtains total alkaloids; The washing lotion of mother liquor and neutralization precipitation merges, and utilizes macroporous resin adsorption (upper prop speed is 0.1% times of resin volume), with 5 times of water washings, then uses 10% ethanol elution; Reclaim ethanol, solid merges with the total alkaloids precipitated above; Dry at 50 ~ 70 DEG C, obtain product.High performance liquid chromatography (HPLC) analytical results shows, total alkaloid content 96% in product, wherein berberine content 48%, other biological alkali content 48%; The yield 92% of Rhizoma Coptidis total alkaloids.
embodiment 2
1 kilogram of coptis fibrous root, adds the sulphuric acid soln of 10 liter 1%, soaks after 12 hours, is warmed up to 60 DEG C and extracts 1 hour, filter; Residue is warmed up to 60 DEG C of extractions three times with the sulphuric acid soln of 10 liter 1% again; Merging first time and the second extracting solution (extract for three times and extract the process being used for next batch raw material four times), separate supernatant liquor after cooling (or filtration obtains supernatant liquor); Supernatant liquor utilizes lime (calcium oxide) to neutralize pH=12, filters, and precipitation utilizes the water washing of 3 times of precipitation capacities to precipitate 1 time; Neutralizer concentrating under reduced pressure 5 times, filters, and filtrate fully stirs rear low temperature (0 DEG C) static 1 hour with about the pH=5 of concentrated hydrochloric acid regulator solution, the sodium-chlor adding 10%; Filter, precipitation suitable quantity of water washs three times, obtains total alkaloids; The washing lotion of mother liquor and neutralization precipitation merges, and utilizes macroporous resin adsorption (upper prop speed is 5% times of resin volume), with 1 times of water washing, then uses 90% ethanol elution; Reclaim ethanol, solid merges with the total alkaloids precipitated above; Dry at 50 ~ 70 DEG C, obtain product.High performance liquid chromatography (HPLC) analytical results shows, total alkaloid content 80% in product, wherein berberine content 40%, other biological alkali content 40%; The yield 93% of Rhizoma Coptidis total alkaloids.
embodiment 3
1 kilogram of coptis lime-ash, adds the sulphuric acid soln of 15 liter 0.1%, soaks after 48 hours, is warmed up to 20 DEG C (if temperature is more than 20 DEG C, can heat up) and extracts 5 hours, filter; Residue is warmed up to 20 DEG C of extractions three times with the sulphuric acid soln of 15 liter 0.1% again; Merging first time and the second extracting solution (extract for three times and extract the process being used for next batch raw material four times), separate supernatant liquor after cooling (or filtration obtains supernatant liquor); Supernatant liquor utilizes lime (calcium oxide) to neutralize pH=6, filters, and precipitation utilizes the water washing of 1 times of precipitation capacity to precipitate 2 times; Neutralizer concentrating under reduced pressure 20 times, filters, and filtrate fully stirs rear low temperature (10 DEG C) static 12 hours with about the pH=3 of concentrated hydrochloric acid regulator solution, the sodium-chlor adding 20%; Filter, precipitation suitable quantity of water washs three times, obtains total alkaloids; The washing lotion of mother liquor and neutralization precipitation merges, and utilizes macroporous resin adsorption (upper prop speed is 2% times of resin volume), with 0.1 times of water washing, then uses 40% ethanol elution; Reclaim ethanol, solid merges with the total alkaloids precipitated above; Dry at 50 ~ 70 DEG C, obtain product.High performance liquid chromatography (HPLC) analytical results shows, total alkaloid content 50% in product, wherein berberine content 25%, other biological alkali content 25%; The yield 95% of Rhizoma Coptidis total alkaloids.
Claims (6)
1. with the coptis and coptis plant for a raw material, adopt the method for sulphuric acid soln soak extraction production high purity Rhizoma Coptidis total alkaloids, described method comprises:
1), raw material prepares
The coptis or coptis fibrous root or coptis lime-ash are removed silt, pulverizes or chopping;
2), soak
Raw material is added aqueous sulfuric acid to soak;
3), extract
After immersion, extract at least twice;
4), feed liquid neutralization
To merge with second time extracting solution first time, filter; Filtrate lime or calcium hydroxide neutralize pH=2 ~ 12 of solution, filter; Residue washes with water again, reclaims the alkaloid that residue is taken away, obtains washings;
5), saltout
By pH=1 ~ 5 of neutralizer with concentrated hydrochloric acid regulator solution; Then, add the sodium-chlor of liquor capacity 1 ~ 20% ratio, 0 ~ 30 DEG C of low temperature puts 1 ~ 48 hour, precipitation total alkaloids;
6), filter and wash
Adopting natural filtration or centrifuging by precipitating the total alkaloids obtained, washing with water simultaneously, being Rhizoma Coptidis total alkaloids;
7), total alkaloids mother liquid disposal
The washings that the mother liquor obtained after precipitation total alkaloids and step 4) stay is merged, according to macroporous resin in the speed of per minute 0.1 ~ 5% times of resin volume, after macroporous resin adsorption, with the water washing resin of 0.1 ~ 5 times of macroporous resin volume, the impurity in removing total alkaloids; Then the ethanol elution of 10 ~ 90%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids;
8), dry
Merge two steps and operate the Rhizoma Coptidis total alkaloids obtained, dry, be high purity Rhizoma Coptidis total alkaloids product.
2. the method for extraction production high purity Rhizoma Coptidis total alkaloids according to claim 1, is characterized in that: for the 4th) neutralizer after the filtration of step, also can carry out pre-concentration, namely carry out concentrating under reduced pressure 1 ~ 20 times, then carry out the 5th step process.
3. the method for extraction production high purity Rhizoma Coptidis total alkaloids according to claim 1 and 2, is characterized in that: the aqueous sulfuric acid (W/V) that raw material is added 3 ~ 15 times of volumes by soak time described 2), concentration is 0.1 ~ 5%, soaks 1 ~ 48 hour.
4. the method for extraction production high purity Rhizoma Coptidis total alkaloids according to claim 1 and 2, is characterized in that: the extraction of described step 3) carries out insulation extraction 0.1 ~ 5 hour after being warmed up to 20 ~ 100 DEG C.
5. the method for extraction production high purity Rhizoma Coptidis total alkaloids according to claim 1 and 2, is characterized in that: described step 3) be extracted as four times, first time and second time extracting solution for the production of product; Third time, extracting solution was for the soak solution as next batch raw material, and directly as primary extracting solution; No. the 4th extracting solution is used for the second time extracting solution of next batch raw material.
6. the method for extraction production high purity Rhizoma Coptidis total alkaloids according to claim 1 and 2, it is characterized in that: the main active ingredient of Rhizoma Coptidis total alkaloids is the Rhizoma Coptidis total alkaloids such as berberine and Berberine, coptisine, epiberberine, palmatine, jateorhizine, the content more than 50% of total alkaloids, the wherein content more than 25% of berberine.
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| CN103751313B (en) * | 2014-01-28 | 2016-08-31 | 西南大学 | A kind of prevention and the Chinese herbal compound preparation for the treatment of fish disease |
| CN104327072A (en) * | 2014-11-25 | 2015-02-04 | 中国药科大学 | Method for extraction and preparation of jatrorrhizine and application of jatrorrhizine in preparation of medicine for prevention and treatment of colon cancer |
| CN104644793A (en) * | 2015-03-20 | 2015-05-27 | 西南大学 | Efficient extraction method of total coptis alkaloids |
| CN105596457A (en) * | 2016-03-01 | 2016-05-25 | 河南中医学院 | Traditional Chinese medicine preparation heart-fire clearing and restlessness relieving tablets for preventing and treating excess-heat anxiety disorder |
| CN106831758B (en) * | 2016-12-20 | 2019-04-19 | 长兴众化生物科技有限公司 | A kind of extracting method of high-purity coptisine |
| CN107126471A (en) * | 2017-05-15 | 2017-09-05 | 北京大学 | Treat pharmaceutical composition of diabetes and its production and use |
| CN110882246B (en) * | 2018-09-08 | 2022-12-23 | 西南大学 | Extraction method and application of coptis alkaloid with different biological activities |
| CN110960583A (en) * | 2018-09-29 | 2020-04-07 | 西南大学 | Pharmaceutical composition for treating acne and application thereof |
| CN109369529B (en) * | 2018-12-29 | 2022-03-04 | 西南大学 | Method for preparing high-purity magnoflorine by taking coptis chinensis extraction mother liquor as raw material, high-purity magnoflorine prepared by method and application |
| CN111686086A (en) * | 2020-07-24 | 2020-09-22 | 焦作福瑞堂制药有限公司 | Compound dandelion and scutellaria tablet and production process thereof |
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| CN101723950B (en) * | 2009-11-26 | 2011-09-28 | 西南大学 | Method for extracting coptisine |
| CN101972320B (en) * | 2010-10-21 | 2012-03-21 | 西南大学 | Method for extracting ferulic acid, chlorogenic acid and other aicd components from coptis chinensis franch |
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