CN101289472A - Process for separating matrine-like total alkaloids form Chinese medicament extract - Google Patents
Process for separating matrine-like total alkaloids form Chinese medicament extract Download PDFInfo
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Abstract
The invention discloses a method for separating total alkaloid of traditional Chinese medicines, in particular a method for separating the matrine type total alkaloid from the extraction solution of traditional Chinese medicines and belongs to the field of traditional Chinese medicines. The method includes the technical proposal as follows: the extraction solution of traditional Chinese medicines is taken; the pH value is adjusted between 1 and 7; the solution is filtered; the filtrate is added to a cation exchange resin column; firstly, water is used for elution and impurity removal; then the acid solution of 0.5 to 15 percent is used for elution; the eluate is collected; the alkali is added for neutralization and then the matrine type total alkaloid is obtained through desalted treatment. The method overcomes the defects of low extraction rate, a large amount of organic solvents, complex process and no mass production, etc., in the prior art and can separate the highly purified matrine type total alkaloid from the extraction solution of traditional Chinese medicines with high efficiency.
Description
Technical field
The present invention relates to a kind of in the extraction and separation method of pharmaceutically active ingredient, particularly relate to a kind of from Chinese medicine extract the alkaloidal method of extraction separation matrine-like total, belong to the field of Chinese medicines.
Background technology
Chinese traditional medicine biology alkali is the class important substance that occurring in nature exists, be separated to kind more than 700 at present, they are maximum class determined curative effects in the Chinese medicine, broad-spectrum effective constituent, especially cancer, hepatopathy and cardiovascular and cerebrovascular, rheumatism major disease etc. there is unique curative effect, be used for antisepsis and anti-inflammation as the Berberine in the coptis, ephedrine in the Chinese ephedra is used to relieving asthma, serpentine in the Radix Rauvolfiae is used for step-down, lycoremine in the short-tube lycoris is effective in cure to poliomyelitis sequela, and contained morphine base is famous analgesic agent in the opium poppy pericarp; Quinine alkali is valuable febrifuge; Capsicine has many physiologically actives and strong and persistent anti-inflammatory analgesic action; It is antitumor etc. that camptothecine in the camplotheca acuminata and the vincristine(VCR) in the Vinca are used for.With matrine and Oxymatyine is the matrine alkaloid of representative, be present in the cassia leguminous plant more, for example Radix Sophorae Tonkinensis, Herba Sophorae alopecuroidis, kuh-seng etc., this Alkaloid can effectively be treated hepatitis B, senile dementia etc., is the very big alkaloid of a class clinical value.
At present, contain the extraction of Chinese traditional medicine biology bases medicinal material, how according to alkaloidal physicochemical property, adopt The suitable solvent such as water, sour water, acid alcohol and alkali alcohol etc., utilize dipping, diacolation, decoction, backflow, technology such as ultrasonic that the alkaloids composition is extracted, extraction process is more perfect, and the alkaloid extraction yield can reach more than 90%.But because the relative content of alkaloid in Chinese medicine lower (most content are 0.01%～1%), certainly will introduce a large amount of impurity constituents during extraction, as a large amount of starch, natural gum, pectin, phlegmatic temperament, pigment etc., giving further discards the dross and selects the essential has brought very big difficulty, thereby real technical bottleneck just is how to be further purified the alkaloid that enrichment extracts.At present, the purification process of widespread use mainly is alkalization back organic solvent extractionprocess and macroporous adsorbent resin method (" Chemistry for Chinese Traditional Medicine ", Xiao Chonghou chief editor,, Shanghai science tech publishing house in 1997 in the alkaloid purifying process; " in the herbal medicine alkaloid extraction with separate ", Cai Yanhua, Sichuan chemical industry, 2005. (1) 39).
Organic solvent extractionprocess is to utilize the lipotropy alkaloid to be dissolved in the lipotropy organic solvent, and the water-soluble character of its salt, the alkaloid soda acid is transformed, utilize organic solvent (commonly used as benzene, trichloromethane, ether etc.) extraction, remove a large amount of impurity, organic solvent extractionprocess is used comparatively extensive, but impurity such as a large amount of neutrality in alkalization back and nonpolar pigment easily are brought into, therefore separation efficiency and purity are lower, and use a large amount of organic solvents (generally extracting 5 times), and (extractor efficient is not high in operation inconvenience, and easily emulsification) not good (organic solvent toxicity is big in security, and inflammable and explosive), be laboratory process, be not suitable for the big production of industry.
The macroporous adsorbent resin isolation technique, effective constituent in the selective adsorption Chinese medicine extract is removed impurity.Compare with technology with traditional impurity-removing method, can dwindle medication dose, improved the quality of preparation, this method has good separation and purification effect to water-soluble flavones, saponin(e etc. preferably, as the ginkgo class preparation commonly used at present and the preparation of ginsenoside etc.But make with extra care for alkaloidal, the deficiency of this law maximum is: at first be the absorption difficulty, last sample soup must be a dilute solution, and basicity will suit, the low then alkaloid of basicity still is an ionization state, the adsorption rate of resin is low, the basicity height, and alkaloid is free type, macromole alkaloid poorly water-soluble and separating out, still can't upper prop, suitable alkaloid scope is very little, and kind is very little; Secondly, the nonpolar electrostatic absorption principle of macroporous adsorbent resin is too poor to the separation selectivity of alkaloid effective ingredient and oil-soluble impurities, and in the solvent elution process owing to there is not a specific eluting solvent, alkaloid and a large amount of oil-soluble impurities often are washed down together, and the total alkaloids purity that final refining obtains is not high.
Also having emerging ion exchange resin isolation technique, is the purpose that reaches separation and purifying by ion exchange reaction.At present the technology that generally adopts in field of Chinese medicines institute is, after will containing alkaloidal solution and crossing post, with ammoniacal liquor or Na0H eluant solution, behind the collection elutriant again with the organic solvent extraction alkaloid; The resin that perhaps will go up sample is with dipping by lye, and then with organic solvent refluxing extraction alkaloid.But this method steps is loaded down with trivial details, organic solvent extraction, resin column is carried out steps such as organic solvent refluxing extraction in industrial very difficult realization, and very low with the efficient of alkali lye wash-out, only stays in the level of prepared in laboratory small sample, also can't realize big production.
More than these methods, ubiquity cost height, organic solvent consumption are big, poor selectivity, total alkaloids purity is low and can't realize deficiency such as big production, therefore, purification technique is still " bottleneck " problem of Chinese medicine separating bio alkali.
Summary of the invention
The purpose of this invention is to provide the alkaloidal method of a kind of safe, low-cost, high efficiency extraction separation matrine-like total.
This goal of the invention realizes by following technology: get and contain the alkaloidal Chinese medicine extract of matrine-like total, adjust pH value 1 to 7, filter, get filtrate and be added on the cation exchange resin column,, use 0.5%～15% acid solution wash-out more earlier with the water elution removal of impurities, collect elutriant, add the alkali neutralization,, promptly get the matrine total alkaloids through desalting treatment.
In above-mentioned technological process, after the extracting solution that will contain total alkaloids transfers to appropriate acidity, alkaloid ionization becomes positively charged ion, nonbasic substances is not ionized, after extracting solution was crossed cation exchange resin column, the hydrogen ion on ionized alkaloid organic ion and the resin column exchanged and is adsorbed on the resin column securely.Here the pH value of extracting solution is unsuitable too high or too low, if too high, it is neutral or alkaline that extracting solution is, and alkaloid can not ionization, also just can not finish the exchange process on the resin; If cross lowly, the hydrogen ion concentration in the extracting solution is too high, has hindered the hydrogen ion on the resin column and has dissociated, and can not finish the resins exchange process well equally, thereby the pH value of finding to adjust extracting solution in the experiment is 1 to 7 to be proper.During with water elution, use be deionized water, to guarantee not introducing new ion interference, those just are not easy to be got off by water elution by the nonbasic substances of resin absorption during wash-out, thus be attracted to resin column on the alkaloid organic ion separated.After this acid solution that adds higher concentration is again carried out wash-out, because the hydrogen ion concentration in the acid solution is very high at this moment, will combine with resin competitively, thereby the alkaloid organic ion that will be adsorbed on the resin column exchanges, be dissolved in the sour elutriant, flow out resin column, finish alkaloidal enrichment process.Afterwards, in elutriant, add alkali and neutralize unnecessary acid,, can obtain matrine total alkaloids that purity is higher again through conventional desalting treatment.
This technological process compared with prior art, technical process is not simple, not with an organic solvent, residual, the alkaloid rate of transform height of no resin monomer composition; Its important contribution also is, has broken ion-exchange capacity order rule, that is: Ca that traditional theory is thought
2+＞K
+≈ NH
4 +＞Na
+＞H
+Just under the influence of this traditional theory, in the alkaloidal ionic exchange resin of matrine-like total all is that alkali lye or ammoniacal liquor carry out wash-out, perhaps earlier with using organic solvent refluxing extraction free alkaloid in theory again with resin column in the alkali lye, and the effect in the practical application is very undesirable and be unsuitable for big production.In technical scheme of the present invention, though hydrionic exchange capacity is the most weak, but by improving hydrionic concentration in the sour elutriant, thereby offset the weak shortcoming of its exchange capacity, simultaneously under acidic conditions, the alkaloid that exchanges is dissolved in the acid solution rapidly, and is rushed out pillar, guarantee alkaloidal elute effect thus.And, carry out wash-out with acid solution, in wash-out, cation exchange resin column is regenerated, thereby can recycle, reduced the process of regenerating resin post behind the alkali lye wash-out, reduced cost.Technology of the present invention has broken through in the prior art traditional concept and the technological process with the alkali lye wash-out fully, obtained beyond thought effect, improved the alkaloidal yield of matrine-like total greatly, making Zeo-karb be used for refining separating matrine-like total alkaloid in industrial production becomes possibility.
Based on above-mentioned technological process, the contriver has carried out further research again, and the parameter of each step of refinement filters out preferred embodiment, and particular content is as follows:
1, the pH value scope of adjustment soup is preferably 2 to 5 before the upper prop, and effect is more obvious.
2, used Zeo-karb can be macroporous type or gel-type strong acid ion exchange resin, can according to circumstances be processed in Hydrogen, sodium type or the ammonium type any when reality is used.
3, the post of used cation exchange resin column footpath there is no a fixed pattern with the ratio of post height, but considers to produce reality, post footpath: post height=1: 5～can obtain best effect at 1: 10 o'clock.
4, the liquor strength to sample on the resin column is that every ml is equivalent to crude drug 0.1～3g, and particular case can determine that if adopt modes such as dipping, diacolation, the soup that obtains will be rarer according to the pre-treatment mode of soup; And if modes such as refluxing extraction, decoction are especially passed through concentration, the concentration of soup will be bigger, but so long as in this scope, can both realize sample.Simultaneously, last sample speed is also adjusted according to the concentration of soup in good time, satisfies substantially at 0.5～5 times of column volume/hour get final product.
5, go up sample loading mode and be typically chosen in from the post upper end upward sample, soup flows through whole pillar by gravity flow power; The contriver finds, if sample on the adverse current, be about to soup sample from the pillar bottom, by certain pressure, make soup fill with whole pillar, thisly go up the maximum exchange efficient that sample loading mode can be brought into play pillar, when also having avoided from the upper end sample since the alkaloid exchange not exclusively take place shift to an earlier date penetration problem.This point also is the creationary discovery of contriver.
6, the used acid solution of wash-out is preferably hydrochloric acid soln or sulphuric acid soln, and its concentration all is preferably 3%～6%.
7, the flow velocity of elutriant is unsuitable too fast or slow excessively during wash-out, if too fast, then the exchange of hydrogen ion and alkaloid organic ion is insufficient, and acid solution is wasted more; If cross slowly, the alkaloid organic ion that then disintegrates down may adsorb back on the resin column again, influences elution efficiency.Experiment finds, elution speed remains on 2～6 times of column volumes/hour be advisable.Further preferred, elution speed remains on 4～6 times of column volumes/hour best.
8, the contriver also finds, improves elution efficiency if think more the highland, can not carry out the acid solution wash-out immediately after the water elution removal of impurities, but is full of acid solution earlier in resin column and leaves standstill more than 2 hours, generally need not surpass 12 hours, carry out wash-out again.Through after leaving standstill, a large amount of alkaloid organic ions are exchanged by hydrogen ion, perhaps are in half absorption, half dissociated state, and carry out wash-out this moment, and the alkaloid concentration effect is obvious, and elution efficiency obviously improves.
9, in order further to improve elution efficiency, can also in the acid solution that wash-out is used, add small amount of N H
4Cl, NaCl or CaCl
2, add-on is unsuitable very few or too much, if very few, does not then have effect; If then easily saltouing because of salt concn is too high influences the solubleness of alkaloid organic ion too much.Experiment finds, in the elutriant with NH
4 +, Na
+Or Ca
2+Be good when concentration is 0.1～1mol/L, further preferred, NH
4 +, Na
+Or Ca
2+Concentration best when being 0.1～0.3mol/L.
10, said desalting method can be the desalination method that dialysis method desalination, membrane filtration are crossed desalination and other various medicine biological field routines in the technology, these methods comparative maturity all at present, and can canalization production.
11, in this method said Chinese medicine extract can be by dipping, diacolation, ultrasonic, microwave or any mode in decocting extract and make, and the solvent that extracts can be in water, sour water, ethanolic soln, the acid ethanol solution any, but all belongs to the conventional extracting method of the present field of Chinese medicines.Distinctive points is, if make with dipping or diacolation method, can directly go up sample; Obtain if extract, also will pass through steps such as alcohol precipitation, filtration or centrifugal removal of impurities, to guarantee the smooth of sample with additive method.
Need to prove that above-mentioned preferred technical parameter can carry out arbitrary combination with basic technology, and all can obtain good effect according to the needs of practical situation, the technical solution problem reaches purpose of the present invention.
Below by the contrast experiment advantage of the present invention is described.
One, experimental program:
Get Radix Sophorae Tonkinensis medicinal material 5000g, add 8 times of amounts of sour water of pH=3, soak a night, diacolation is collected percolate to do not have a precipitation with the silicotungstic acid inspection till, merges percolate, and is centrifugal, supernatant liquor; Supernatant liquor is five parts, carries out alkaloidal separation by following five kinds of methods respectively and purify:
(1) ion exchange resin+acid solution wash-out: supernatant liquor is regulated pH=3, on handled strong cation-exchanging resin 001 * 7 (Hydrogen well, blade diameter length ratio is 1: 8), last sample speed be 3 times of column volumes/hour, there is precipitation to stop to go up sample with the silicotungstic acid inspection to effluent liquid, it is colourless substantially that water is eluted to elutriant, use 3% hydrochloric acid soln wash-out again, elution speed be 4 times of column volumes/hour the speed wash-out, elutriant has precipitation the time to begin to receive with the silicotungstic acid inspection, receive elutriant to do not have with the silicotungstic acid inspection precipitation up to, merge elutriant, be neutralized to neutrality with sodium hydroxide, desalination (standby), drying gets total alkaloids of subprostrate sophora root.
(2) the acid solution wash-out of ion exchange resin+salt: supernatant liquor is regulated pH=3, on handled strong cation-exchanging resin 001 * 7 (Hydrogen well, blade diameter length ratio is 1: 8), last sample speed be 3 times of column volumes/hour, there is precipitation to stop to go up sample with the silicotungstic acid inspection to effluent liquid, water is not eluted to when elutriant has color substantially and stops, and 0.5% hydrochloric acid soln with 2% calcium chloride soaks resin again.Use 0.5% hydrochloric acid soln wash-out of 2% calcium chloride again, elution speed be 4 times of column volumes/hour, elutriant begins to receive when with the silicotungstic acid inspection precipitation being arranged, receive elutriant to do not have with the silicotungstic acid inspection precipitation up to, merge elutriant, be neutralized to about pH=7 desalination (standby) with calcium hydroxide, concentrate drying gets total alkaloids of subprostrate sophora root.
(3) ion exchange resin+refluxing extraction: supernatant liquor is regulated pH=3, on handled strong cation-exchanging resin 001 * 7 (Hydrogen, blade diameter length ratio are 1: 8) well, last sample speed be 3 times of column volumes/hour, there is precipitation to stop to go up sample with the silicotungstic acid inspection to effluent liquid, water is not eluted to when elutriant has color substantially and stops wash-out, and resin by pouring out in the post, is put in the porcelain dish and dried, it is an amount of to add 10% ammoniacal liquor, stir, touched damp, be not advisable but do not touch with one's hand with hand.This resin is put in the apparatus,Soxhlet's,, chloroform solution is added anhydrous Na with chloroform refluxing extraction 2 hours
2SO
4After the dehydration, reclaim chloroform, the dry total alkaloids of subprostrate sophora root that gets to the dried molassed pulpous state.
(4) macroporous adsorbent resin method: supernatant liquor is regulated pH=10, on the DF01 type macroporous adsorbent resin handled well, last sample speed be 4 times of column volumes/hour, have precipitation to stop to go up sample with the silicotungstic acid inspection to effluent liquid, water is eluted to and stops wash-out when elutriant does not have color substantially.With alcohol-water (70: 30) is eluent, with 2.5 times of column volumes/hour speed carry out wash-out, elutriant has precipitation the time to begin to receive with the silicotungstic acid inspection, receive elutriant to do not have with the silicotungstic acid inspection precipitation up to, merge elutriant, reclaim ethanol, drying gets total alkaloids of subprostrate sophora root.
(5) organic solvent extractionprocess: supernatant liquor is regulated pH=10, divide three extractions with 10 times of amount chloroforms earlier, measure ethyl acetate extractions three times with 10 times again, merge all extraction liquids, evaporate to dryness gets total alkaloids of subprostrate sophora root.
Two, the result calculates: distinguish the weight of five kinds of technology gained of weighing total alkaloids, and be divided by with the medicinal material amount, get the yield of total alkaloids; Adopt the quantivative approach of acid base titration respectively, five kinds of method gained total alkaloidss are carried out assay, calculate the purity of total alkaloids.
Three, result's contrast, see the following form:
The effect assessment table of five kinds of technologies
By above comparing result as seen, technical scheme of the present invention can solve deficiency of the prior art, and improve significantly product quality, reduce cost, improve security and producing feasibility, the present invention has reached goal of the invention.
Technical scheme of the present invention is suitable for the refining purifying of matrine-like total alkaloid valid target.Kuh-seng is the root of leguminous plants kuh-seng (SopHora flavescens Ait.), record in 2005 editions one one 141 pages of Chinese Pharmacopoeia pharmacopeia, have another name called " bitter bone ", " phoenix ginseng ", " river ginseng ", " wild Chinese scholartree " etc., have effects such as heat-clearing and damp-drying drug, desinsection, diuresis.Radix Sophorae Tonkinensis is the dry root and rhizome of leguminous plants sophora tonkinensis Gapnep SopHora tonkinensis Gagnep., records in 2005 editions one one 19 pages of Chinese Pharmacopoeia pharmacopeia, has another name called " mountain soybean root ", " Herba Astragali Melilotoidis " etc., has clearing heat and detoxicating, effect such as detumescence relieve sore throat etc.Herba Sophorae alopecuroidis is cassia leguminous plant Herba Sophorae alopecuroidis (SopHora alopecuroides L.) herb or root or a seed, has another name called Root of Foxtail-like sophora, effects such as tool clearing heat and promoting diuresis, pain relieving, desinsection.Root of Vetchleaf Sophora is the root of leguminous plants Root of Vetchleaf Sophora SopHora viciifolia Hance, has another name called " staple acupuncture ", " wolf's fang thorn ", has clearing heat and cooling blood, effect such as inducing diuresis and reducing edema, clearing heat and detoxicating.Sophora moocroftiana(Wall is the fruit of pulse family Sophora moocroftiana(Wall SopHoramoorcroftiana (Wall.) Benth.ex Baker, has the effect of eliminating inflammation and expelling toxin.Above-mentioned five kinds of medicinal materials all derive from the pulse family Sophora, and contained chemical ingredients is also substantially the same, and mostly is matrine alkaloid.Studies show that, their total alkaloidss separately are its main efficient parts, comprise matrine (Matrine) in the kuh-seng, Oxymatyine (Oxymatrine), sophor-anol (SopHoranol), N-Methylcytisine (N-methylcytisine), dehydrogenation matrine (SopHocarpine), Anagyrine (Anagyrine) etc.; Matrine in the Radix Sophorae Tonkinensis (Matrine), Oxymatyine (Oxyma-trine), rhombinin (Anagyrine), methylcytisine (Methylcytisne), sophocarpine (SopHocarpine); Matrine in the Herba Sophorae alopecuroidis (Matrine), Oxymatyine (Oxymatrinel), sophocarpine (SopHocarpine), Sophocarpidin (OxysopHocarpine), sophoramine (SopHoramine), sophorine (SopHoridine), Lemannine (Lehmannine), ALOPERINE (Alopefine); Matrine in the Root of Vetchleaf Sophora (Matrine), Oxymatyine (Oxyma-trine) etc.; Matrine in the Sophora moocroftiana(Wall (Matrine), Oxymatyine alkaloid components such as (Oxyma-trine).Clinical matrine total alkaloids is controlled the treatment that agent has been used for hepatitis B etc., has shown good curative effect.Confirm through a large amount of tests, the alkaloidal technology of Zeo-karb sour water wash-out matrine-like total, have that cost is low, organic solvent consumption less, the selectivity height, total alkaloids purity is high and help realizing advantage such as the big production of industry, for a brand-new platform has been created in the R﹠D and production of Chinese medicine matrine-like total alkaloid formulations.
Embodiment
Embodiment 1:
Get kuh-seng medicine materical crude slice 1000g, boiling 2 times, each 10 times of amounts decocted 2 hours, merged decoction liquor, centrifugal, regulate pH=3, centrifugal, supernatant liquor is with 4 times of column volumes/hour by Zeo-karb (001 * 7, Hydrogen, blade diameter length ratio 1: 8), being washed to effluent liquid does not have color, adds 3% sulfuric acid wash-out, elution speed be 2 times of column volumes/hour, collect elutriant, check negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide to alkaloid, desalination, the filtrate concentrate drying gets Radix Sophorae Flavescentis total alkaloids.
Embodiment 2:
Get Radix Sophorae Tonkinensis medicine materical crude slice 1000g, the sour water diacolation that adds pH=5, merge the percolate thin up to 10000ml, centrifugal, regulate pH=1, centrifugal, supernatant liquor is with 5 times of column volumes/hour by Zeo-karb (001 * 12, the sodium type, blade diameter length ratio 1: 5), being washed to effluent liquid does not have color, use 0.5% hydrochloric acid soln wash-out again, elution speed be 4 times of column volumes/hour, soaked behind 2 times of column volumes of wash-out 5 hours, be eluted to alkaloid again and check negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), collect this part elutriant, be neutralized to neutrality with calcium hydroxide, desalination, the filtrate concentrate drying gets total alkaloids of subprostrate sophora root.
Embodiment 3:
Get Sophora moocroftiana(Wall medicine materical crude slice 5kg, add 70% ethanol ultrasonic extraction twice, add 5 times of amounts at every turn, ultrasonic 0.5 hour, united extraction liquid, centrifugal, reclaim ethanol, add water to 5000ml, regulate pH=2, centrifugal, supernatant liquor is with 2 times of column volumes/hour by last Zeo-karb (001 * 10, sodium type, blade diameter length ratio 1: 7), being washed to effluent liquid does not have color, uses 6% the hydrochloric acid soln (CaCl that contains 1mol/L again
2) wash-out, elution speed be 5 times of column volumes/hour, collect elutriant, check negative (effluent liquid drips 10% silicotungstic acid does not have precipitation) to alkaloid, be neutralized to neutrality with sodium hydroxide, desalination, the filtrate concentrate drying gets the Sophora moocroftiana(Wall total alkaloids.
Embodiment 4:
Get Root of Vetchleaf Sophora medicine materical crude slice 10kg, boiling 2 times, each 10 times of amounts decocted 2 hours, merge decoction liquor, filter, it is 1.1 (60 ℃) that filtrate is concentrated into relative density, and adding ethanol to concentration is 70%, leave standstill, supernatant liquor reclaims ethanol, adds water to 3000ml, regulates pH=4, centrifugal, supernatant liquor is with 3 times of column volumes/hour by last Zeo-karb (011 * 6, ammonia type, blade diameter length ratio 1: 9), be washed to effluent liquid and do not have color, use 15% sulphuric acid soln wash-out again, elution speed be 6 times of column volumes/hour, collect elutriant, to alkaloid inspection negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide, desalination, the filtrate concentrate drying gets the Root of Vetchleaf Sophora total alkaloids.
Embodiment 5:
Get Root of Vetchleaf Sophora medicine materical crude slice 10kg, boiling 2 times, each 10 times of amounts decocted 2 hours, merge decoction liquor, filter, it is 1.1 (60 ℃) that filtrate is concentrated into relative density, and adding ethanol to concentration is 70%, leave standstill, supernatant liquor reclaims ethanol, adds water to 5000ml, regulates pH=5, centrifugal, supernatant liquor is with 3 times of column volumes/hour by last Zeo-karb (D001 * 4, Hydrogen, blade diameter length ratio 1: 10), be washed to effluent liquid and do not have color, use 3% hydrochloric acid soln wash-out again, elution speed be 3 times of column volumes/hour, collect elutriant, to alkaloid inspection negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide, desalination, the filtrate concentrate drying gets the Root of Vetchleaf Sophora total alkaloids.
Embodiment 6:
Get kuh-seng medicine materical crude slice 10kg, boiling 2 times, each 10 times of amounts decocted 2 hours, merge decoction liquor, filter, it is 1.1 (60 ℃) that filtrate is concentrated into relative density, and adding ethanol to concentration is 70%, leave standstill, supernatant liquor reclaims ethanol, adds water to 4000ml, regulates pH=4, centrifugal, supernatant liquor is with 0.5 times of column volume/hour by last Zeo-karb (001 * 18, Hydrogen, blade diameter length ratio 1: 6), be washed to effluent liquid and do not have color, use 0.5% sulphuric acid soln (sodium-chlor that contains 0.1mol/L) wash-out again, elution speed be 5 times of column volumes/hour, collect elutriant, to alkaloid inspection negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide, desalination, the filtrate concentrate drying gets Radix Sophorae Flavescentis total alkaloids.
Embodiment 7:
Get Sophora moocroftiana(Wall medicine materical crude slice 10kg, boiling 2 times, each 10 times of amounts decocted 2 hours, merge decoction liquor, filter, it is 1.1 (60 ℃) that filtrate is concentrated into relative density, and adding ethanol to concentration is 70%, leave standstill, supernatant liquor reclaims ethanol, adds water to 10000ml, regulates pH=3, centrifugal, supernatant liquor is with 3 times of column volumes/hour by last Zeo-karb (001 * 5, Hydrogen, blade diameter length ratio 1: 8), be washed to effluent liquid and do not have color, use 15% hydrochloric acid soln (calcium chloride that contains 0.3mol/L) wash-out again, elution speed be 6 times of column volumes/hour, collect elutriant, to alkaloid inspection negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide, desalination, the filtrate concentrate drying gets the Sophora moocroftiana(Wall total alkaloids.
Embodiment 8:
Get Root of Vetchleaf Sophora medicine materical crude slice 1000g, boiling 2 times, each 10 times of amounts decocted 2 hours, merge decoction liquor, filter, it is 1.1 (60 ℃) that filtrate is concentrated into relative density, and adding ethanol to concentration is 70%, leave standstill, supernatant liquor reclaims ethanol, adds water to 1000ml, regulates pH=3, centrifugal, supernatant liquor is with 3 times of column volumes/hour by last Zeo-karb (001 * 5, Hydrogen, blade diameter length ratio 1: 8), be washed to effluent liquid and do not have color, use 6% sulphuric acid soln wash-out again, elution speed be 4 times of column volumes/hour, collect elutriant, to alkaloid inspection negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide, desalination, the filtrate concentrate drying gets the Root of Vetchleaf Sophora total alkaloids.
Embodiment 9:
Get Radix Sophorae Tonkinensis medicine materical crude slice 2000g, the hydrochloric acid soln that adds pH=3, microwave extraction 2 times adds 5 times of volume microwave extraction 0.5 hour at every turn, filters, the filtrate thin up is to 1600ml, regulate pH=6, centrifugal, supernatant liquor is with 2 times of column volumes/hour by last Zeo-karb (001 * 15, Hydrogen, blade diameter length ratio 1: 6), being washed to effluent liquid does not have color, uses 5% hydrochloric acid soln (ammonia chloride that contains 0.2mol/L) wash-out again, elution speed be 5 times of column volumes/hour, collect elutriant, check negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide to alkaloid, desalination, the filtrate concentrate drying gets total alkaloids of subprostrate sophora root.
Embodiment 10:
Get Herba Sophorae alopecuroidis medicine materical crude slice 5kg, add twice of 70% ethanol ultrasonic extraction, add 5 times of amounts at every turn, ultrasonic 0.5 hour, united extraction liquid, centrifugal, reclaim ethanol, add water to 5000ml, regulate pH=7, centrifugal, supernatant liquor is so that 2 times of column volumes/hour by last large pores cation exchange resin, being washed to effluent liquid does not have color, uses 4% sulphuric acid soln (ammonia chloride of 0.6mol/L) wash-out again, elution speed be 5 times of column volumes/hour, collect elutriant, check negative (effluent liquid drips 10% silicotungstic acid does not have precipitation), be neutralized to neutrality with sodium hydroxide to alkaloid, desalination, the filtrate concentrate drying gets total alkaloid of sophora alopecuroide.
Claims (13)
1, a kind of from Chinese medicine extract the alkaloidal method of separating matrine-like total, it is characterized in that this method is: get and contain the alkaloidal Chinese medicine extract of matrine-like total, adjust pH value 1 to 7, filter, get filtrate and be added on the cation exchange resin column, earlier with the water elution removal of impurity, use 0.5%～15% acid solution wash-out again, collect elutriant, add the alkali neutralization, through desalting treatment, promptly get the matrine total alkaloids.
2, the alkaloidal method of separating matrine-like total as claimed in claim 1 is characterized in that the preceding pH value scope of adjusting soup of upper prop is 2 to 5.
3, the alkaloidal method of separating matrine-like total as claimed in claim 1 is characterized in that used Zeo-karb can be macroporous type or gel-type strong acid ion exchange resin.
4, the alkaloidal method of separating matrine-like total as claimed in claim 3 is characterized in that the post footpath of used cation exchange resin column: post height=1: 5～1: 10.
5, the alkaloidal method of separating matrine-like total as claimed in claim 1 is characterized in that in this method that the concentration of sample soup is that every ml is equivalent to crude drug 0.1～3g, last sample speed be 0.5～5 times of column volume/hour.
6, the alkaloidal method of separating matrine-like total as claimed in claim 5 is characterized in that sample loading mode is preferably sample on the adverse current.
7, the alkaloidal method of separating matrine-like total as claimed in claim 1 is characterized in that wash-out is used in this method acid solution is 3%～6% hydrochloric acid soln or 3%～6% sulphuric acid soln.
8, the alkaloidal method of separating matrine-like total as claimed in claim 7, it is characterized in that elution speed be 2～6 times of column volumes/hour.
9, the alkaloidal method of separating matrine-like total as claimed in claim 8, it is characterized in that elution speed be 4～6 times of column volumes/hour.
10, the alkaloidal method of separating matrine-like total as claimed in claim 1 is characterized in that after the water elution removal of impurities, can be full of wash-out earlier with acid solution and left standstill 2～12 hours in resin column, carries out wash-out again.
11, the alkaloidal method of separating matrine-like total as claimed in claim 7 is characterized in that can also adding in the acid solution that wash-out uses the NH of 0.1～1mol/L
4Cl, NaCl or CaCl
2
12, the alkaloidal method of separating matrine-like total as claimed in claim 11 is characterized in that the concentration of salt is preferably 0.1～0.3mol/L in the acid solution.
13, the matrine total alkaloids of any one described method preparation among the claim 1-12.
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| CN103422351A (en) * | 2013-08-02 | 2013-12-04 | 吴江市七都镇庙港雅迪针织制衣厂 | Woolen sweater treating liquid containing abietic acid polyoxyethylene ester |
| CN104415573A (en) * | 2013-09-10 | 2015-03-18 | 中国科学院大连化学物理研究所 | Method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract |
| CN106018642A (en) * | 2016-06-27 | 2016-10-12 | 柳州市妇幼保健院 | SPE-HPLC (Solid Phase Extraction-High Performance Liquid Chromatography) method for measuring content of matrine in LeShu washing liquor |
| CN111138433A (en) * | 2020-01-16 | 2020-05-12 | 西藏德康生物科技有限公司 | Method for extracting and purifying matrine from sophora moorcroftianain |
| CN113713008A (en) * | 2021-09-10 | 2021-11-30 | 西藏自治区农牧科学院畜牧兽医研究所 | Sophora Moorcroftiana alkaloid extraction process |
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2007
- 2007-04-18 CN CNA2007100143359A patent/CN101289472A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422351A (en) * | 2013-08-02 | 2013-12-04 | 吴江市七都镇庙港雅迪针织制衣厂 | Woolen sweater treating liquid containing abietic acid polyoxyethylene ester |
| CN103422351B (en) * | 2013-08-02 | 2015-05-20 | 苏州爱立方服饰有限公司 | Woolen sweater treating liquid containing abietic acid polyoxyethylene ester |
| CN104415573A (en) * | 2013-09-10 | 2015-03-18 | 中国科学院大连化学物理研究所 | Method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract |
| CN104415573B (en) * | 2013-09-10 | 2017-03-22 | 中国科学院大连化学物理研究所 | Method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract |
| CN106018642A (en) * | 2016-06-27 | 2016-10-12 | 柳州市妇幼保健院 | SPE-HPLC (Solid Phase Extraction-High Performance Liquid Chromatography) method for measuring content of matrine in LeShu washing liquor |
| CN111138433A (en) * | 2020-01-16 | 2020-05-12 | 西藏德康生物科技有限公司 | Method for extracting and purifying matrine from sophora moorcroftianain |
| CN113713008A (en) * | 2021-09-10 | 2021-11-30 | 西藏自治区农牧科学院畜牧兽医研究所 | Sophora Moorcroftiana alkaloid extraction process |
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