CN104644793A - Efficient extraction method of total coptis alkaloids - Google Patents
Efficient extraction method of total coptis alkaloids Download PDFInfo
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Abstract
The invention belongs to the technical field of extraction of active ingredients of traditional Chinese medicines, and particularly relates to an efficient extraction method of total coptis alkaloids. The efficient extraction method aims at solving the technical problems that the purity and the yield of the total coptis alkaloids extracted in the prior art are not high. The efficient extraction method of the total coptis alkaloids is characterized in that the efficient extraction method comprises the following steps of 1) smashing raw materials, 2) pretreating the raw materials, 3) percolating, 4) neutralizing percolation liquid, 5) concentrating, 6) salting out, 7) filtering and washing, 8) treating total alkaloid mother liquid, and 9) drying. The efficient extraction method is simple to operate and low in energy consumption; the cost of industrial production is lowered greatly; the extraction yield of the total coptis alkaloids reaches above 98%; and main active ingredients of the total coptis alkaloids are berberine hydrochloride, namely berberin, coptisine, epiberberine, palmatine, jateorhizine, etc.
Description
Technical field
The invention belongs to active ingredient of Chinese herbs extractive technique field, be specifically related to the highly effective extraction method of Rhizoma Coptidis biology total alkali.
Background technology
Rhizoma Coptidis begins to be loaded in Shennong's Herbal, is classified as top grade.Rhizoma Coptidis bitter in the mouth, cold in nature, there is the function of pathogenic fire purging, removing toxic substances, heat clearing away, dampness.For dysphoria with smothery sensation coma, vexed insomnia, damp and hot feeling of fullness, vomiting, stomachache dysentery, conjunctival congestion toxic swelling, aphtha of the mouth and tongue, eczema, scald, haematemesis, epistaxis etc.Modern pharmacy result of study shows, Rhizoma Coptidis main active is Rhizoma Coptidis total alkaloids, mainly comprises (" Chinese Pharmacopoeias " 2010 editions) such as berberine (berberine), palmatine, coptisine, epiberberine and jateorhizine; Rhizoma Coptidis (element) has the pharmacologically active widely such as blood fat reducing and blood sugar lowering.Nearest research finds, except berberine, Rhizoma Coptidis related alkaloids active component (coptisine, palmatine etc.) also has the effect such as blood fat reducing and blood sugar lowering (Hou Hong etc., Rhizoma Coptidis alkaloid anti-hyperlipidemia and atherosclerosis experimentation, time precious traditional Chinese medical science traditional Chinese medicines, 2011,22 (10): 2462.); Also find simultaneously, highly purified Rhizoma Coptidis alkaloid safety is very high, and Rhizoma Coptidis alkaloid crude product will cause the safety issues (JunYi 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, Rhizoma Coptidis price is very expensive, and the extraction ratio and the yield that improve Rhizoma Coptidis total alkaloids are the keys 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, with soak by water, upper macroporous resin purification, washing, aquiferous ethanol eluting, 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 ratio of the total alkaloidss such as Rhizoma Coptidis directly uses soak by water, berberine is poor; On Rhizoma Coptidis alkaloid after resin, during eluting, resin is difficult to 100% regeneration, and resin utilization rate is not high; When reclaiming ethanol, ethanol inevitably loses and high energy consumption etc., causes cost increase etc.; This Technology is owing to using Rhizoma Coptidis, and the extraction ratio of Rhizoma Coptidis alkaloid is lower (less than 90%).
Chinese patent literature (200810069671.8) reports a kind of coptis chinensis total alkaloid extracting technique technology, mainly comprises: raw material (Rhizoma Coptidis or Rhizoma Coptidis fibrous root or leaf of Rhizoma Coptidis)---pulverizes (as do not needed to pulverize for Rhizoma Coptidis fibrous root or leaf of Rhizoma Coptidis)---add the soak with sulphuric acid of appropriate 0.01 ~ 10%---intensification extraction four times---pre-concentration---purification---sodium chloride and high-valency metal salt precipitation---filtration---oven dry---Rhizoma Coptidis total alkaloids product.The main active of product is the Rhizoma Coptidis effective ingredient 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 solution 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 adsorbent (as active hargil, silica gel, active carbon or various macroporous resins etc.) to purify, and the operation such as recrystallization, technique is comparatively complicated, and production cost is high; This technique Rhizoma Coptidis and also etc. not pulverizing, alkaloidal extraction ratio not high (less than 90%); High temperature reflux under acid condition, easily causes active component loss etc., is also to cause one of reason that yield is not high.
Chinese patent literature (02103880.5) reports extraction process and the novelty teabag thereof of Rhizoma Coptidis total alkaloids, mainly comprise: Rhizoma Coptidis water soaking and time ultrasonic Treatment, total alkaloids extraction is carried out under warm macerating 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 chloride again, leave standstill, then the precipitate in extracting solution is collected by sucking filtration or centrifuge dripping, precipitate is dried, precipitate after oven dry is pulverized, and can obtain Rhizoma Coptidis total alkaloids hydrochlorate 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 solution, use Rhizoma Coptidis, the yield of total alkaloids is not high yet simultaneously.
Chinese patent literature (201110053453.7) reports a kind of method utilizing polyamide separation and purification Rhizoma Coptidis alkaloid, mainly comprise: Rhizoma Coptidis crude extract polyamide is upper polyamide column after mixing sample, with dichloromethane eluent or the mixed solvent gradient elution with dichloromethane and methanol, with thin layer chromatography inspection stream part, merge same stream part, drying, namely separablely obtains seven alkaloids such as berberine, palmatine, coptisine, Columbamine, jateorhizine, magnoflorine, Groenlandcine.What this Technology was separated is Rhizoma Coptidis alkaloid monomer, and owing to relating to the very large dichloromethane equal solvent of toxicity in separation and purification process, safety is difficult to ensure.
Chinese patent literature (200810218824.0) reports Rhizoma Coptidis total alkaloids and is preparing the application in treating diabetic complications medicine, mainly comprises: 1) Rhizoma Coptidis is ground into coarse powder; 2) 5-10 times amount 60-80% ethanol is by Rhizoma Coptidis coarse powder reflux, extract, 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 lime cream respectively, filters, adjusts pH1 ~ 2 respectively, add sodium chloride and make salinity reach 10%, shake up with hydrochloric acid, leaves standstill, obtains Rhizoma Coptidis total alkaloids.This technique does not relate to the problems such as the recovery of Rhizoma Coptidis total alkaloids in the rear mother solution of Rhizoma Coptidis total alkaloids precipitation yet; Rhizoma Coptidis is ground into coarse powder, and the extraction ratio of total alkaloids is not high.
Chinese patent literature (201310357973.6) reports a kind of high-purity coptis chinensis total alkaloid extracting technique technology, the production method of its total alkaloids is: Rhizoma Coptidis or Rhizoma Coptidis fibrous root or Rhizoma Coptidis lime-ash, pulverize (as do not needed to pulverize for Rhizoma Coptidis fibrous root or Rhizoma Coptidis lime-ash), add the soak with sulphuric acid of 0.1 ~ 5%, intensification extraction four times, filter, calcium oxide (or calcium hydroxide) neutralizes, and filters and washing precipitation, pre-concentration, acid adjustment, Sodium chloride deposit, filters, disposing mother liquor alkaloid, precipitation is dried, Rhizoma Coptidis total alkaloids product.This technique can obtain highly purified Rhizoma Coptidis total alkaloids, and has reclaimed the total alkaloids in mother solution, and yield is higher; But this technique is appointed and is so had the following disadvantages: 1., raw material pulverizing fineness is inadequate, and the extraction ratio of total alkaloids is not high (less than 95%); If grinding particle size is too thin, directly filter very difficult; 2., adopt temperature rising reflux to extract, not only energy consumption is high, and high temperature extraction under acid condition, part effective ingredient (as jateorhizine) easily decomposes.
-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 to extract and purification process, mainly comprise: Rhizoma Coptidis decoction pieces adds the sulfuric acid solution of 8 times amount 1.5%, decoct 3 times, each 40min; Rhizoma Coptidis extract Ca (OH) 2 regulates pH5 ~ 6, sucking filtration, it is that every mL is containing 0.24g crude drug that filtrate heating is concentrated into concentration, sucking filtration, filtrate salt adding acid for adjusting pH 1.5 ~ 2, adds 5% sodium chloride solution and makes dissolving, hold over night in refrigerator, sucking filtration, filtering residue vacuum drying (50 DEG C), collects purified.Rhizoma Coptidis total alkaloids extraction ratio 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.Owing to adopting Rhizoma Coptidis decoction pieces extracting directly, yield is not ideal enough.
In sum, although the Technology extracting Rhizoma Coptidis total alkaloids is very many, but, ubiquity total alkaloids yield is not high, or purity is undesirable, complex process, or relate to toxic solvent in the course of processing, or under acid condition, high temperature extraction causes the problems such as effective ingredient decomposed.
In the art, extraction ratio refers to the biological alkali number be dissolved into from Rhizoma Coptidis in solution, the product volume that yield finally obtains after being through extraction operation, decomposes the amount referring to active ingredient breaks down loss in Rhizoma Coptidis leaching process.One of index of the extraction most critical of the middle active component of the valuable medicinals such as Rhizoma Coptidis (value is more than 50 yuan/Kg) is yield: if the active component in raw material can not fully be transferred in extracting solution, certainly affect yield; Active component is transferred in solution very abundant, decomposes, yield also can be caused to reduce in extraction or following process process; Active component is transferred in solution very abundant, also undecomposed in extraction or following process process, but can there is various loss in subsequent processes, and some losses can be very large, and final yield also can be caused to decline.
And from the report of prior art, prior art does not all consider that the decomposition of active component in alkaloidal extraction ratio and the course of processing in Rhizoma Coptidis is on the impact etc. of yield, mainly there is blind spot in research: namely many research workers did not carry out systematic analysis, not the grinding particle size of systematic study Rhizoma Coptidis raw material and the relation of extraction ratio; Study Rhizoma Coptidis grinding particle size and the extraction ratio relation with regard to the rate of filtration (percolation speed), and solution accordingly; The decomposition of systematic study leaching process Active principals is not on the impact of yield; Namely and do not know alkaloid in which step have lost, thus up to the present there is not yet various relevant parameter to the systematic study report improving Rhizoma Coptidis total alkaloids yield.
Summary of the invention
The technical problem to be solved in the present invention first has Rhizoma Coptidis total alkaloids to extract moderate purity and the not high problem of yield.
Technical scheme of the present invention is the highly effective extraction method of Rhizoma Coptidis biology total alkali, comprises the steps:
1) raw material pulverizing: Rhizoma Coptidis, Cortex Phellodendri, Radix Berberidis or Mahonia fortunei (Lindl.) Fedde are crushed to 10 ~ 150 orders;
2) pretreatment of raw material: to step 1) add 0.001 ~ 5 times to the additive of raw material fine powder volume in the raw material fine powder that obtains, then adding 2 ~ 4 times of raw material fine powder volumetric concentrations is that the aqueous sulfuric acid of 0.1 ~ 3% (V/V) stirs, for subsequent use;
3) percolation: the solution modulated proceeds in percolator, soaks at 0 ~ 50 DEG C after 0.1 ~ 24 hour, starts percolation; Percolation speed be 0.01 ~ 1.0 times of Rhizoma Coptidis fine powder volume/hour; The percolate of the front 8 times of raw material fine powder volumes collected is used for following process, and the percolate of the 6 times of raw material fine powder volumes collected subsequently is for the process of next group raw material;
4) neutralization of percolate: the pH2 ~ 10 percolate Calx of the front 8 times of volumes collected or calcium hydroxide being neutralized solution, filters; Residue uses the water washing 1 ~ 3 time (object of washing is the alkaloid that recovery residue is taken away) of 0.1 ~ 3 times of level of residue again, merging filtrate and washing liquid:
5) concentrated: by the neutralizer concentrating under reduced pressure 1 ~ 20 times after merging; Cooled and filtered, obtains clarifying concentrated solution;
6) saltout: the pH1 ~ 5 clear liquor concentrated hydrochloric acid after concentrated being regulated solution; Then, add the sodium chloride of solution weight 1 ~ 20% ratio, 0 ~ 30 DEG C of low temperature puts 1 ~ 48 hour, precipitation total alkaloids;
7) filter and wash: the total alkaloids obtained will be precipitated and adopt natural filtration or centrifugal filtration, and wash with water simultaneously, be Rhizoma Coptidis total alkaloids:
8) total alkaloids mother liquid disposal: by the mother solution after precipitation total alkaloids according to macroporous resin in the speed of 0.1 ~ 5% times of resin volume per minute, 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;
9) dry: merge the 7th and the 8th liang of step and operate the Rhizoma Coptidis total alkaloids obtained, dry at 50 ~ 80 DEG C, be high-purity Rhizoma Coptidis total alkaloids product.
Concrete, step 1) in pulverizing order number be 25 ~ 100 orders.
Preferably, step 1) in, described raw material is Rhizoma Coptidis.
Concrete, described Rhizoma Coptidis is Rhizoma Coptidis fibrous root, Rhizoma Coptidis lime-ash or Rhizoma Coptidis stem and leaf.
Concrete, step 2) described in filter aid be silica gel, Muscovitum, perlite, kieselguhr, river sand, pearlife or glass bead closed perlite.
Preferably, described filter aid is perlite.
Most preferred, described perlite is closed perlite.
Concrete, step 2) in the consumption of filter aid be: the volume of filter aid is 3 ~ 4 times of raw material fine powder.
Concrete, step 3) in, the solution modulated proceeds in percolator, soaks and start percolation in 6 ~ 12 hours later under room temperature.
Concrete, step 4) middle adjustment pH 4 ~ 7.
Preferably, Rhizoma Coptidis is crushed to 100 orders; Filter aid is perlite, and its consumption is 2 times of raw material fine powder volume; Raw material fine powder soaks 24 and as a child started percolation afterwards; Percolate calcium oxide adjusts pH5.
Concrete, the operation of described method is as follows:
1) raw material pulverizing: Rhizoma Coptidis, Cortex Phellodendri, Radix Berberidis or Mahonia fortunei (Lindl.) Fedde are crushed to 100 orders;
2) pretreatment of raw material: to step 1) add 0 ~ 5 times to the perlite of raw material fine powder volume in the raw material fine powder that obtains, then adding 2 ~ 4 times of raw material fine powder volumetric concentrations is that the aqueous sulfuric acid of 0.1%V/V stirs, for subsequent use;
3) percolation: the solution modulated proceeds in percolator, soaked after 24 hours, started percolation; Percolation speed be 0.01 ~ 1.0 times of Rhizoma Coptidis fine powder volume/hour; The percolate of the front 8 times of raw material fine powder volumes collected is used for following process, and the percolate of the 6 times of raw material fine powder volumes collected subsequently is for the process of next group raw material;
4) neutralization of percolate: the pH5 percolate Calx of the front 8 times of volumes collected or calcium hydroxide being neutralized solution, filters; Residue uses the water washing 1 time of 3 times of level of residue again, merging filtrate and washing liquid:
5) concentrated: by the neutralizer concentrating under reduced pressure 20 times after merging; Cooled and filtered, obtains clarifying concentrated solution;
6) saltout: the pH5 clear liquor concentrated hydrochloric acid after concentrated being regulated solution; Then, add the sodium chloride of solution weight 20% ratio, 0 DEG C of low temperature puts 1 hour, precipitation total alkaloids;
7) filter and wash: the total alkaloids obtained will be precipitated and adopt natural filtration or centrifugal filtration, and wash with water simultaneously, be Rhizoma Coptidis total alkaloids:
8) total alkaloids mother liquid disposal: by the mother solution after precipitation total alkaloids according to macroporous resin in the speed of 0.1% times of resin volume per minute, after macroporous resin adsorption, with the water washing resin of 0.1 times of macroporous resin volume, the impurity in removing total alkaloids; Then the ethanol elution of 90%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids;
9) dry: merge the 7th and the 8th liang of step and operate the Rhizoma Coptidis total alkaloids obtained, dry at 50 ~ 70 DEG C, be high-purity Rhizoma Coptidis total alkaloids product.
In the present invention, after the famous and precious raw material powders such as Rhizoma Coptidis are broken into fine grained, obviously can increase the extraction ratio of active component, the production cost of extract can be reduced.Add filter aid, percolation speed can be significantly improved, meet industrial needs; Meanwhile, additive can improve the extraction ratio of active component.Adopt sulfuric acid solution extract at low temperature (percolation), avoid high temperature reflux under acid condition; Extracting solution recycling calcium oxide (calcium hydroxide) neutralization removing sulphuric acid; and then concentrating under reduced pressure; for unstability active component (active component as phenolic hydroxy group), there is fabulous protective effect, be conducive to the ultimate yield improving active component.
Beneficial effect of the present invention: the inventive method to the extraction rate reached of Rhizoma Coptidis total alkaloids to more than 98%; The main active 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.Leaching process does not always have the loss of active component; Simple to operate, energy consumption is low, 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 80%, biological value is higher, and safety is better; The extract obtained is the desirable feedstock of blood fat reducing, blood sugar lowering and fat-reducing.
The Rhizoma Coptidis total alkaloids that the present invention obtains, have the effects such as more preferably blood sugar lowering, blood fat reducing and fat-reducing than single Rhizoma Coptidis.Product of the present invention (Rhizoma Coptidis total alkaloids) can, as the succedaneum of the products such as Rhizoma Coptidis, Rhizoma Coptidis concentrated product, berberine, may be used for treating diabetes, hyperlipidemia, obesity and cardiovascular disease.
Detailed description of the invention
The comparative study result of embodiment 1 Rhizoma Coptidis grinding particle size and extraction ratio relation
1., Rhizoma Coptidis is crushed to 150 orders
By Rhizoma Coptidis 100g, be crushed to 150 orders; By Rhizoma Coptidis fine powder, add the perlite of 0.5 times of volume, then add 3 times of volumetric concentrations be 1% aqueous sulfuric acid (V/V) stir; The solution modulated proceeds in percolator, soaks after 6 hours at 15 DEG C, starts percolation, percolation speed be 0.1 times of volume/hour; Collect the percolate of 8 times of volumes, obtain 800 milliliters.The content of sample analysis Rhizoma Coptidis total alkaloids, calculates extraction ratio.
Percolate calcium hydroxide neutralizes the pH=5 of solution, filters; Residue uses the water washing 1 time of 1 times of level of residue again, reclaims the alkaloid that residue is taken away, obtains cleaning mixture; Solution and washing liquid thereof after neutralization, concentrating under reduced pressure 10 times, cooled and filtered, obtains clarifying concentrated solution; Clear liquor after concentrated concentrated hydrochloric acid regulates the pH=3 of solution, and then, add the sodium chloride of liquor capacity 10% ratio, 20 DEG C of low temperature put 24 hours; By precipitating, the total alkaloids obtained is centrifugal, simultaneously with 10 ml water washings, is Rhizoma Coptidis total alkaloids.
Mother solution after precipitation total alkaloids and washing of precipitate liquid are merged, according to macroporous resin in the speed of 1% times of resin volume per minute, after macroporous resin adsorption, with the water washing resin of 2 times of macroporous resin volumes, the impurity in removing total alkaloids; Then the ethanol elution of 60%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids.
Merge two steps and operate the Rhizoma Coptidis total alkaloids obtained, dry, be high-purity Rhizoma Coptidis total alkaloids product, obtain total alkaloids 15 grams.Sample analysis alkaloid, calculated yield, the results are shown in Table 1.
2., Rhizoma Coptidis is crushed to 100 orders
Except Rhizoma Coptidis raw material pulverizing granularity difference, all the other operations are same 1..
3., Rhizoma Coptidis is crushed to 50 orders
Except Rhizoma Coptidis raw material pulverizing granularity difference, all the other operations are same 1..
4., Rhizoma Coptidis is crushed to 10 orders
Except Rhizoma Coptidis raw material pulverizing granularity difference, all the other operations are same 1..
The extraction ratio of table 1 Rhizoma Coptidis grinding particle size and total alkaloids and the relation research of yield
Remarks: theoretical content × 100% of total alkaloids in extraction ratio=liquor capacity × concentration ÷ Rhizoma Coptidis
Rhizoma Coptidis total alkaloids is berberine, coptisine, palmatine, epiberberine, Simultaneous Determinat ion sum.Alkaloid concentrations and content HPLC methods analyst.
Can see from table 1, along with the fineness pulverized increases, the extraction ratio of Rhizoma Coptidis total alkaloids increases, and after especially fineness reaches 50 orders, extraction ratio increases sharply; Extracting increase is the important leverage improving yield.Visible, being pulverized by material thin as much as possible, is the important measures improving Rhizoma Coptidis total alkaloids yield.
The contrast experiment of embodiment 2 Rhizoma Coptidis grinding particle size and filtration (percolation) speed
1., Rhizoma Coptidis is crushed to 150 orders
By Rhizoma Coptidis 100g, be crushed to 150 orders; Add in Rhizoma Coptidis fine powder 3 times of volumetric concentrations be 1% aqueous sulfuric acid (V/V) stir; The solution modulated proceeds in percolator, starts percolation, measures percolation speed, the results are shown in Table 2.Collect the percolate of 8 times of volumes, obtain 800 milliliters.The content of sample analysis Rhizoma Coptidis total alkaloids, calculates extraction ratio.
2., Rhizoma Coptidis is crushed to 100 orders
Except Rhizoma Coptidis raw material pulverizing granularity is different unexpected, all the other operations are same 1..
3., Rhizoma Coptidis is crushed to 50 orders
Except Rhizoma Coptidis raw material pulverizing granularity is different unexpected, all the other operations are same 1..
4., Rhizoma Coptidis is crushed to 10 orders
Except Rhizoma Coptidis raw material pulverizing granularity is different unexpected, all the other operations are same 1..
Table 2, Rhizoma Coptidis grinding particle size and filtration (percolation) length velocity relation are studied
Liquid amasss × concentration ÷ Rhizoma Coptidis in theoretical content × 100% of total alkaloids
Rhizoma Coptidis total alkaloids is berberine, coptisine, palmatine, epiberberine, Simultaneous Determinat ion sum.Alkaloid concentrations and content are analyzed.
Can see from table 2, increase with the fineness doing to pulverize, the rate of filtration of solution declines rapidly; When Rhizoma Coptidis pulverize granularity lower than 50 orders after, percolation speed is very poor; When Rhizoma Coptidis grinding particle size is lower than 100 order, solution substantially can not percolation.Visible, along with the increase of granularity, although the extraction ratio of Rhizoma Coptidis total alkaloids increases, time due to percolation speed too slow, in fact cannot percolation (filtration).
Embodiment 3 additive connects contrast experiment's research of fine powder percolation (filtration) rate to 150 icteric sclera
1., 150 icteric sclera connect fine powder
100g is crushed in 150 object Rhizoma Coptidis fine powders, add 3 times of volumetric concentrations be 1% aqueous sulfuric acid (V/V) stir; The solution modulated proceeds in percolator, starts percolation, measures percolation speed, the results are shown in Table 3.Collect the percolate of 8 times of volumes, obtain 800 milliliters.The content of sample analysis Rhizoma Coptidis total alkaloids, calculates extraction ratio.
2., 150 icteric sclera connect the silica gel (or perlite) of fine powder+1% Rhizoma Coptidis fine powder weight
Except the silica gel (or perlite) of interpolation 1%, all the other operations are same 1..
3., 150 icteric sclera connect the silica gel (or perlite) of fine powder+10%
Except the silica gel (or perlite) of interpolation 10%, all the other operations are same 1..
4., 150 icteric sclera connect the silica gel (or perlite) of fine powder+100%
Except the silica gel (or perlite) of interpolation 100%, all the other operations are same 1..
Table 3 additive connects the research of fine powder percolation (filtration) rate to 150 icteric sclera
Remarks: theoretical content × 100% of total alkaloids in extraction ratio=liquor capacity × concentration ÷ Rhizoma Coptidis
Rhizoma Coptidis total alkaloids is berberine, coptisine, palmatine, epiberberine, Simultaneous Determinat ion sum.Alkaloid concentrations and content are analyzed.
Can see from table 3, add the percolation speed that filter aid not only can significantly improve Rhizoma Coptidis fine powder, and can extraction ratio be increased.This may be relevant with increase percolation effect.
Embodiment 4 the technology of the present invention and the contrast experiment of prior art in extraction ratio and yield
1., the technology of the present invention (100 order)
By Rhizoma Coptidis 100g, be crushed to 100 orders; By Rhizoma Coptidis fine powder, add the perlite of 0.5 times of volume, then add 3 times of volumetric concentrations be 1% aqueous sulfuric acid (V/V) stir; The solution modulated proceeds in percolator, soaks after 6 hours at 15 DEG C, starts percolation, percolation speed be 0.1 times of volume/hour; Collect the percolate of 8 times of volumes, obtain 800 milliliters.The content of sample analysis Rhizoma Coptidis total alkaloids, calculates extraction ratio.
Percolate calcium hydroxide neutralizes the pH=5 of solution, filters; Residue uses the water washing 1 time of 1 times of level of residue again, reclaims the alkaloid that residue is taken away, obtains cleaning mixture; Solution and washing liquid thereof after neutralization, concentrating under reduced pressure 10 times, cooled and filtered, obtains clarifying concentrated solution; Clear liquor after concentrated concentrated hydrochloric acid regulates the pH=3 of solution, and then, add the sodium chloride of liquor capacity 10% ratio, 20 DEG C of low temperature put 24 hours; By precipitating, the total alkaloids obtained is centrifugal, simultaneously with 10 ml water washings, is Rhizoma Coptidis total alkaloids.
Mother solution after precipitation total alkaloids and washing of precipitate liquid are merged, according to macroporous resin in the speed of 1% times of resin volume per minute, after macroporous resin adsorption, with the water washing resin of 2 times of macroporous resin volumes, the impurity in removing total alkaloids; Then the ethanol elution of 60%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids.
Merge two steps and operate the Rhizoma Coptidis total alkaloids obtained, dry, be high-purity Rhizoma Coptidis total alkaloids product, obtain total alkaloids 15 grams.Sample analysis alkaloid, calculated yield, the results are shown in Table 4.
2., the technology of the present invention (100 order)
Originally before operating in percolation, be first warmed up to 50 DEG C of insulations 1 hour, all the other all operations are same 1..
3., the technology of the present invention (100 order)
Originally before operating in percolation, be first warmed up to 70 DEG C of insulations 1 hour, all the other all operations are same 1..
4., the technology of the present invention (100 order)
Originally before operating in percolation, be first warmed up to 90 DEG C of insulations 1 hour, all the other all operations are same 1..
5., the technology of the present invention (100 order)
Originally before operating in percolation, be first warmed up to 100 DEG C of insulations 1 hour, all the other all operations are same 1..
6., patented technology (201310357973.6)
Rhizoma Coptidis 100g is removed silt, pulverizes; Add 5 times of volumes in raw material, concentration be 1% aqueous sulfuric acid (V/V), soak 6 hours; After immersion, be warmed up to 100 DEG C, insulation extraction 3 hours; First time and second time extracting solution merge, and obtain solution 800 milliliters.The extraction ratio of sample analysis Rhizoma Coptidis total alkaloids.
To merge with second time extracting solution first time, filter; Filtrate neutralizes the pH=5 of solution with calcium hydroxide, filters; Residue uses the water washing 1 time of 1 times of level of residue again, reclaims the alkaloid that residue is taken away, obtains cleaning mixture; Solution and washing liquid thereof after neutralization, concentrating under reduced pressure 10 times, cooled and filtered, obtains clarifying concentrated solution; Clear liquor after concentrated concentrated hydrochloric acid regulates the pH=3 of solution, and then, add the sodium chloride of liquor capacity 10% ratio, 20 DEG C of low temperature put 24 hours; By precipitating, the total alkaloids obtained is centrifugal, simultaneously with 10 ml water washings, is Rhizoma Coptidis total alkaloids.
Mother solution after precipitation total alkaloids and washing of precipitate liquid are merged, according to macroporous resin in the speed of 1% times of resin volume per minute, after macroporous resin adsorption, with the water washing resin of 2 times of macroporous resin volumes, the impurity in removing total alkaloids; Then the ethanol elution of 60%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids.
Merge two steps and operate the Rhizoma Coptidis total alkaloids obtained, dry, be high-purity Rhizoma Coptidis total alkaloids product, obtain total alkaloids 13 grams.Sample analysis alkaloid, calculated yield.
7., technical literature (new Chinese medicine and clinical pharmacology.2012，23(2)：208)
Rhizoma Coptidis decoction pieces 100g, adds the sulfuric acid solution of 8 times amount 1.5%, decocts 3 times, each 40min; Merge extractive liquid, obtains solution 800 milliliters.The extraction ratio of sample analysis Rhizoma Coptidis total alkaloids.
Rhizoma Coptidis extract is with Ca (OH)
2regulate pH5 ~ 6, sucking filtration, it is that every mL contains 0.24g crude drug, sucking filtration that filtrate heating is concentrated into concentration, filtrate salt adding acid for adjusting pH 1.5 ~ 2, adds 5% sodium chloride solution and makes dissolving, hold over night in refrigerator, sucking filtration, filtering residue vacuum drying (50 DEG C), collects purified.Rhizoma Coptidis total alkaloids extraction ratio about 93%, total alkaloids yield about 60%, total alkaloids purity about 84%.
The extraction ratio of table 4 Rhizoma Coptidis total alkaloids and yield
Remarks: theoretical content × 100% of total alkaloids in extraction ratio=liquor capacity × concentration ÷ Rhizoma Coptidis
Rhizoma Coptidis total alkaloids is berberine, coptisine, palmatine, epiberberine, Simultaneous Determinat ion sum.Alkaloid concentrations and content are analyzed.
Can see from table 4, the extraction ratio of this Technology Rhizoma Coptidis total alkaloids and yield are all obviously better than patented technology (201310357973.6) and document (new Chinese medicine and clinical pharmacology.2012,23 (2): 208) technology reported.The result of study that contrast the technology of the present invention is incubated rear percolation at different temperatures finds, after percolation temperature is more than 50 DEG C, extraction ratio and yield all decline with the rising making temperature; Further analysis (HPLC analysis) also finds, the mainly jateorhizine changed under acid condition etc. are containing phenolic hydroxyl group Alkaloid, and jateorhizine has good hypolipidemic activity, be one of the important active component of Rhizoma Coptidis (Hao Wu, etc.The antihypercholesterolemic effect of jatrorrhizine isolated from RhizomaCoptidis。Phytomedicine。21(2014)：1373–1381)。These results of study show, Rhizoma Coptidis alkaloid is less stable in acid condition, and under acid condition, high temperature extraction causes the decomposition of Rhizoma Coptidis alkaloid, are one of major reasons affecting extraction ratio and yield.
The Rhizoma Coptidis total alkaloids that embodiment 5 the present invention obtains and existing berberine are in safety and the contrast for the treatment of in relevant disease
1., subchronic toxicity testing
Test material is Rhizoma Coptidis total alkaloids (content 80%), berberine (content 95%), the Rhizoma Coptidis total alkaloids crude product that the present invention obtains
(total alkaloid content 40%).
Subchronic toxicity testing method reference-natural drug (Chinese medicine) new drug research guideline ‖ carries out: 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, the results are shown in Table 5.
Table 5 Rhizoma Coptidis total alkaloids is on the impact of rat liver function
| Sample | Glutamate pyruvate transaminase (ALT) (U/L) | Glutamic oxaloacetic transaminase, GOT (AST) (U/L) |
| Normal group | 34.20±4.40 | 126.34±7.69 |
| Rhizoma Coptidis total alkaloids group | 34.06±2.60 | 122.66±5.60 |
| Berberine group | 33.90±1.86 | 127.32±12.99 |
| Rhizoma Coptidis total alkaloids crude product group | 39.62±9.35 | 168.04±18.42 |
Can see from table 5, 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 adverse effect.The result of this result and bibliographical information is similar (Jun Yi etc.Safetyevaluation of main alkaloids from Rhizoma Coptidis.Journal of Ethnopharmacology, 2013.145:303-310).
2., hypolipidemic activity experiment
Test material is that Rhizoma Coptidis total alkaloids (total alkaloid content 80%), berberine (content 95%), Rhizoma Coptidis total alkaloids crude product that the present invention obtains are (total
Alkaloid 40%).
Lipid-lowering test method reference-natural drug (Chinese medicine) new drug research guideline ‖ carries out: Golden Hamster is divided into 5 groups, and 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 matched 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, the results are shown in Table 6.
Table 6 Rhizoma Coptidis total alkaloids lipid-lowering effect compares
Can see from table 6, 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 safety 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.
Embodiment 6 adopts the inventive method to extract Rhizoma Coptidis biology total alkali
1 kilogram of Rhizoma Coptidis is crushed to 10 orders, adds 1 gram of silica gel as additive, then adds the sulfuric acid solution (V/V) of 2 liter 3%, soaks 0.1 hour, with the speed percolation of 1L/h at 50 DEG C; Collect 8L percolation solution for the production of product, continue to collect the percolation of 6L percolate for next group raw material; Percolate utilizes Calx (calcium oxide) to neutralize pH=2, filters, and precipitation utilizes the water washing of 0.1 times of precipitation capacity to precipitate 3 times, and filtrate and washing liquid merge, concentrating under reduced pressure 1 times; After cooling, filter, clarification concentrated solution utilizes concentrated hydrochloric acid to regulate about the pH=1 of solution, and the sodium chloride 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; Mother solution and washing liquid merge, and utilize macroporous resin adsorption (upper prop speed is 0.1% times of resin volume), with 5 times of water washings, then use 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) analysis result shows, the extraction ratio 91.5% of total alkaloids; Total alkaloid content 90% in product, wherein berberine content 45%, other biological alkali content 45%; The yield 86% of Rhizoma Coptidis total alkaloids.
Embodiment 7 adopts the inventive method to extract Rhizoma Coptidis biology total alkali
1 kilogram of Rhizoma Coptidis is crushed to 100 orders, adds 2000 grams of closed perlite powder as additive, then adds the sulfuric acid solution (V/V) of 4 liter 0.1%, soaks 24 hours, with the speed percolation of 10mL/h at 0 DEG C; Collect 8L percolation solution for the production of product, continue to collect the percolation of 6L percolate for next group raw material; Percolate utilizes Calx (calcium oxide) to neutralize pH=10, filters, and precipitation utilizes the water washing of 3 times of precipitation capacities to precipitate 1 time, and filtrate and washing liquid merge, concentrating under reduced pressure 20 times; After cooling, filter, clarification concentrated solution utilizes concentrated hydrochloric acid to regulate about the pH5 of solution, and the sodium chloride adding 20% fully stirs rear room temperature (0 DEG C) static 1 hour; Filter, precipitation suitable quantity of water is washed once, obtains total alkaloids; Mother solution and washing liquid merge, and utilize macroporous resin adsorption (upper prop speed is 0.1% times of resin volume), with 0.1 times of water washing, then use 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) analysis result shows, the extraction ratio 99.7% of total alkaloids; Total alkaloid content 50% in product, wherein berberine content 25%, other biological alkali content 25%; The yield 98.1% of Rhizoma Coptidis total alkaloids.
Embodiment 8 adopts the inventive method to extract Rhizoma Coptidis biology total alkali
1 kilogram of Rhizoma Coptidis is crushed to 150 orders, adds 5000 grams of kieselguhr as additive, then adds the sulfuric acid solution (V/V) of 3 liter 0.5%, soaks 12 hours, with the speed percolation of 100mL/h at 10 DEG C; Collect 8L percolation solution for the production of product, continue to collect the percolation of 6L percolate for next group raw material; Percolate utilizes Calx (calcium oxide) to neutralize pH=5, filters, and precipitation utilizes the water washing of 1 times of precipitation capacity to precipitate 2 times, and filtrate and washing liquid merge, concentrating under reduced pressure 10 times; After cooling, filter, clarification concentrated solution utilizes concentrated hydrochloric acid to regulate about the pH=3 of solution, and the sodium chloride adding 10% fully stirs rear room temperature (10 DEG C) static 12 hours; Filter, precipitation suitable quantity of water is washed once, obtains total alkaloids; Mother solution and washing liquid merge, and utilize macroporous resin adsorption (upper prop speed is 0.5% times of resin volume), with 1 times of water washing, then use 60% 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) analysis result shows, the extraction ratio 99.1% of total alkaloids; Total alkaloid content 70% in product, wherein berberine content 35%, other biological alkali content 35%; The yield 97.3% of Rhizoma Coptidis total alkaloids.
Embodiment 9 adopts the inventive method to extract Rhizoma Coptidis biology total alkali
1 kilogram of Rhizoma Coptidis is crushed to 50 orders, adds 100 grams of river sands as additive, then adds the sulfuric acid solution (V/V) of 3 liter 1%, soaks 6 hours, with the speed percolation of 300mL/h at 20 DEG C; Collect 8L percolation solution for the production of product, continue to collect the percolation of 6L percolate for next group raw material; Percolate utilizes Calx (calcium oxide) to neutralize pH=7, filters, and precipitation utilizes the water washing of 0.5 times of precipitation capacity to precipitate 2 times, and filtrate and washing liquid merge, concentrating under reduced pressure 5 times; After cooling, filter, clarification concentrated solution utilizes concentrated hydrochloric acid to regulate about the pH=4 of solution, and the sodium chloride adding 5% fully stirs rear room temperature (20 DEG C) static 24 hours; Filter, precipitation suitable quantity of water is washed once, obtains total alkaloids; Mother solution and washing liquid merge, and utilize macroporous resin adsorption (upper prop speed is 0.2% times of resin volume), with 1 times of water washing, then use 30% 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) analysis result shows, the extraction ratio 97.3% of total alkaloids; Total alkaloid content 80% in product, wherein berberine content 40%, other biological alkali content 40%; The yield 95.8% of Rhizoma Coptidis total alkaloids.
Embodiment 10 adopts the inventive method to extract Cortex Phellodendri biology total alkali
1 kilogram of Cortex Phellodendri is crushed to 50 orders, adds 100 grams of river sands as additive, then adds the sulfuric acid solution (V/V) of 3 liter 1%, soaks 6 hours, with the speed percolation of 300mL/h at 20 DEG C; Collect 8L percolation solution for the production of product, continue to collect the percolation of 6L percolate for next group raw material; Percolate utilizes Calx (calcium oxide) to neutralize pH=7, filters, and precipitation utilizes the water washing of 0.5 times of precipitation capacity to precipitate 2 times, and filtrate and washing liquid merge, concentrating under reduced pressure 5 times; After cooling, filter, clarification concentrated solution utilizes concentrated hydrochloric acid to regulate about the pH=4 of solution, and the sodium chloride adding 5% fully stirs rear room temperature (20 DEG C) static 24 hours; Filter, precipitation suitable quantity of water is washed once, obtains total alkaloids; Mother solution and washing liquid merge, and utilize macroporous resin adsorption (upper prop speed is 0.2% times of resin volume), with 1 times of water washing, then use 30% 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) analysis result shows, the extraction ratio 97.1% of total alkaloids; Total alkaloid content 80% in product, wherein berberine content 75%, other biological alkali content 5%.
Embodiment 11 adopts the inventive method to extract Radix Berberidis biology total alkali
1 kilogram of Radix Berberidis is crushed to 50 orders, adds 100 grams of river sands as additive, then adds the sulfuric acid solution (V/V) of 3 liter 1%, soaks 6 hours, with the speed percolation of 300mL/h at 20 DEG C; Collect 8L percolation solution for the production of product, continue to collect the percolation of 6L percolate for next group raw material; Percolate utilizes Calx (calcium oxide) to neutralize pH=7, filters, and precipitation utilizes the water washing of 0.5 times of precipitation capacity to precipitate 2 times, and filtrate and washing liquid merge, concentrating under reduced pressure 5 times; After cooling, filter, clarification concentrated solution utilizes concentrated hydrochloric acid to regulate about the pH=4 of solution, and the sodium chloride adding 5% fully stirs rear room temperature (20 DEG C) static 24 hours; Filter, precipitation suitable quantity of water is washed once, obtains total alkaloids; Mother solution and washing liquid merge, and utilize macroporous resin adsorption (upper prop speed is 0.2% times of resin volume), with 1 times of water washing, then use 30% 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) analysis result shows, the extraction ratio 97.5% of total alkaloids; Total alkaloid content 80% in product, wherein berberine content 70%, other biological alkali content 10%.
Claims (9)
1. the highly effective extraction method of Rhizoma Coptidis biology total alkali, is characterized in that: comprise the steps:
1) raw material pulverizing: Rhizoma Coptidis, Cortex Phellodendri, Radix Berberidis or Mahonia fortunei (Lindl.) Fedde are crushed to 10 ~ 150 orders;
2) pretreatment of raw material: to step 1) add 0 ~ 5 times to the filter aid of raw material fine powder volume in the raw material fine powder that obtains, then adding 2 ~ 4 times of raw material fine powder volumetric concentrations is that the aqueous sulfuric acid of 0.1 ~ 3%V/V stirs, for subsequent use;
3) percolation: the solution modulated proceeds in percolator, soaked after 0.1 ~ 24 hour, started percolation; Percolation speed be 0.01 ~ 1.0 times of Rhizoma Coptidis fine powder volume/hour; The percolate of the front 8 times of raw material fine powder volumes collected is used for following process, and the percolate of the 6 times of raw material fine powder volumes collected subsequently is for the process of next group raw material;
4) neutralization of percolate: the pH2 ~ 10 percolate Calx of the front 8 times of volumes collected or calcium hydroxide being neutralized solution, filters; Residue uses the water washing 1 ~ 3 time of 0.1 ~ 3 times of level of residue again, merging filtrate and washing liquid:
5) concentrated: by the neutralizer concentrating under reduced pressure 1 ~ 20 times after merging; Cooled and filtered, obtains clarifying concentrated solution;
6) saltout: the pH1 ~ 5 clear liquor concentrated hydrochloric acid after concentrated being regulated solution; Then, add the sodium chloride of solution weight 1 ~ 20% ratio, 0 ~ 30 DEG C of low temperature puts 1 ~ 48 hour, precipitation total alkaloids;
7) filter and wash: the total alkaloids obtained will be precipitated and adopt natural filtration or centrifugal filtration, and wash with water simultaneously, be Rhizoma Coptidis total alkaloids:
8) total alkaloids mother liquid disposal: by the mother solution after precipitation total alkaloids according to macroporous resin in the speed of 0.1 ~ 5% times of resin volume per minute, 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;
9) dry: merge the 7th and the 8th liang of step and operate the Rhizoma Coptidis total alkaloids obtained, dry at 50 ~ 80 DEG C, be high-purity Rhizoma Coptidis total alkaloids product.
2. the method for claim 1, is characterized in that: step 1) in, described raw material is Rhizoma Coptidis.Concrete, described Rhizoma Coptidis is Rhizoma Coptidis fibrous root, Rhizoma Coptidis lime-ash or Rhizoma Coptidis stem and leaf.
3. method as claimed in claim 2, is characterized in that: step 1) in pulverizing order number be 25 ~ 100 orders.
4. the method as described in claims 1 to 3, is characterized in that: step 2) described in filter aid be silica gel, Muscovitum, perlite, kieselguhr, river sand, pearlife or glass bead closed perlite.
Preferably, described filter aid is perlite.
Most preferred, described perlite is closed perlite.
5. the method as described in any one of Claims 1 to 4, is characterized in that: step 2) in the consumption of filter aid be: the volume of filter aid is 3 ~ 4 times of raw material fine powder.
6. the method as described in any one of Claims 1 to 5, is characterized in that: step 3) in, the solution modulated proceeds in percolator, soaks and start percolation in 6 ~ 12 hours later under room temperature.
7. the method as described in any one of claim 1 ~ 6, is characterized in that: step 4) middle adjustment pH 4 ~ 7.
8. the method as described in any one of claim 4 ~ 7, is characterized in that: Rhizoma Coptidis is crushed to 100 orders; Filter aid is perlite, and its consumption is 2 times of raw material fine powder volume; Raw material fine powder soaks 24 and as a child started percolation afterwards; Percolate calcium oxide adjusts pH5.
9. method as claimed in claim 8, is characterized in that:
1) raw material pulverizing: Rhizoma Coptidis, Cortex Phellodendri, Radix Berberidis or Mahonia fortunei (Lindl.) Fedde are crushed to 100 orders;
2) pretreatment of raw material: to step 1) add 0 ~ 5 times to the perlite of raw material fine powder volume in the raw material fine powder that obtains, then adding 2 ~ 4 times of raw material fine powder volumetric concentrations is that the aqueous sulfuric acid of 0.1%V/V stirs, for subsequent use;
3) percolation: the solution modulated proceeds in percolator, soaked after 24 hours, started percolation; Percolation speed be 0.01 ~ 1.0 times of Rhizoma Coptidis fine powder volume/hour; The percolate of the front 8 times of raw material fine powder volumes collected is used for following process, and the percolate of the 6 times of raw material fine powder volumes collected subsequently is for the process of next group raw material;
4) neutralization of percolate: the pH5 percolate Calx of the front 8 times of volumes collected or calcium hydroxide being neutralized solution, filters; Residue uses the water washing 1 time of 3 times of level of residue again, merging filtrate and washing liquid:
5) concentrated: by the neutralizer concentrating under reduced pressure 20 times after merging; Cooled and filtered, obtains clarifying concentrated solution;
6) saltout: the pH5 clear liquor concentrated hydrochloric acid after concentrated being regulated solution; Then, add the sodium chloride of solution weight 20% ratio, 0 DEG C of low temperature puts 1 hour, precipitation total alkaloids;
7) filter and wash: the total alkaloids obtained will be precipitated and adopt natural filtration or centrifugal filtration, and wash with water simultaneously, be Rhizoma Coptidis total alkaloids:
8) total alkaloids mother liquid disposal: by the mother solution after precipitation total alkaloids according to macroporous resin in the speed of 0.1% times of resin volume per minute, after macroporous resin adsorption, with the water washing resin of 0.1 times of macroporous resin volume, the impurity in removing total alkaloids; Then the ethanol elution of 90%, after reclaiming ethanol, obtains Rhizoma Coptidis total alkaloids;
9) dry: merge the 7th and the 8th liang of step and operate the Rhizoma Coptidis total alkaloids obtained, dry at 50 ~ 70 DEG C, be high-purity Rhizoma Coptidis total alkaloids product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675761A (en) * | 2016-02-03 | 2016-06-15 | 成都中医药大学 | HPLC method for simultaneously determining contents of four alkaloid components in cortex berberidis |
| CN106831758A (en) * | 2016-12-20 | 2017-06-13 | 长兴众化生物科技有限公司 | A kind of extracting method of high-purity coptisine |
| CN113144015A (en) * | 2020-10-23 | 2021-07-23 | 重庆伊士腾生物科技有限公司 | Application of product of xianglian or combination of product of xianglian and antibiotic in anti-helicobacter pylori medicine |
| CN113244315A (en) * | 2020-02-12 | 2021-08-13 | 重庆伊士腾生物科技有限公司 | Preparation method and application of anti-Hp coptis Chinese medicine preparation |
| CN115745783A (en) * | 2023-01-04 | 2023-03-07 | 赣州奥润吉新材料有限公司 | Zero-emission stannous oxalate production method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103393780A (en) * | 2013-08-16 | 2013-11-20 | 西南大学 | Extraction method of high-purity coptis total alkaloid |
| CN104418852A (en) * | 2013-08-30 | 2015-03-18 | 西南大学 | Extracting method and application of high-purity coptisine |
-
2015
- 2015-03-20 CN CN201510124240.7A patent/CN104644793A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103393780A (en) * | 2013-08-16 | 2013-11-20 | 西南大学 | Extraction method of high-purity coptis total alkaloid |
| CN104418852A (en) * | 2013-08-30 | 2015-03-18 | 西南大学 | Extracting method and application of high-purity coptisine |
Non-Patent Citations (1)
| Title |
|---|
| 宋小妹: "《中药化学》", 31 August 2012, 湖南科学技术出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675761A (en) * | 2016-02-03 | 2016-06-15 | 成都中医药大学 | HPLC method for simultaneously determining contents of four alkaloid components in cortex berberidis |
| CN106831758A (en) * | 2016-12-20 | 2017-06-13 | 长兴众化生物科技有限公司 | A kind of extracting method of high-purity coptisine |
| CN113244315A (en) * | 2020-02-12 | 2021-08-13 | 重庆伊士腾生物科技有限公司 | Preparation method and application of anti-Hp coptis Chinese medicine preparation |
| CN113144015A (en) * | 2020-10-23 | 2021-07-23 | 重庆伊士腾生物科技有限公司 | Application of product of xianglian or combination of product of xianglian and antibiotic in anti-helicobacter pylori medicine |
| CN115745783A (en) * | 2023-01-04 | 2023-03-07 | 赣州奥润吉新材料有限公司 | Zero-emission stannous oxalate production method |
| CN115745783B (en) * | 2023-01-04 | 2023-09-19 | 赣州奥润吉新材料有限公司 | Production method of zero-emission stannous oxalate |
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