CN101791340B - Method for purifying active ingredients of compound Naodesheng - Google Patents
Method for purifying active ingredients of compound Naodesheng Download PDFInfo
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Abstract
The invention discloses a method for purifying active ingredients of compound Naodesheng. The method comprises the following steps: firstly dividing raw materials of the compound Naodesheng into two parts for screening, wherein the first part comprises sanchi, kudzuvine root, hawthorn fruit and Szechuan lovage rhizome, and the second part comprises safflower; carrying out extraction, concentration, vacuum filtration, concentration, absorption by resin and elution on the two parts, then extracting and purifying for obtaining purified eluate of the two parts, merging, decompressing, concentrating and drying for obtaining the active ingredients of the compound Naodesheng. The method for purifying the compound Naodesheng can effectively remove impurities without efficacy, ensure the yield, relatively improve the content of the active ingredients, improve the efficacy of the drug and realize very high using value.
Description
Technical field
The present invention relates to medicine purification field, be specifically related to a kind of purification process of active ingredients of compound Naodesheng.
Background technology
Compound Naodesheng is effective Chinese medicine compound, 1979 through the Heilongjiang Province Department of Public Health approval produce NAODESHENG ball and NAODESHENG PIAN Chinese patent medicine kind, nineteen ninety-five is put into Chinese Pharmacopoeia; Reprinting Chinese Pharmacopoeia in 2000 and 2005 all records continuously; Form by Radix Notoginseng 78g, Rhizoma Chuanxiong 78g, Flos Carthami 91g, Radix Puerariae 261g, Fructus Crataegi (enucleation) 157g five kinds of Chinese medicine, have blood circulation promoting and blood stasis dispelling, dredging the meridian; The effect of consciousness-restoring and orifice-opening; Be used for cerebral arteriosclerosis, illness such as ischemia apoplexy and apoplexy sequela, evident in efficacy.
The pharmacological action of each flavour of a drug of NAODESHENG mainly contains: each flavour of a drug all has the effect of blood circulation promoting and blood stasis dispelling in the NAODESHENG compound recipe.Modern pharmacological research shows: Radix Notoginseng total arasaponins and flavones ingredient have inhibition and analgesic activity to the central nervous system; Cardiovascular system there are effects such as arrhythmia, coronary artery dilating, increase coronary flow, anti-experimental character myocardial ischemia; Blood system there are hemostasis and anticoagulant effect; Also has blood fat reducing, antioxidation, defying age, effects such as enhancing immunity.Compositions such as ligustrazine in the Rhizoma Chuanxiong and ferulic acid have coronary artery dilating, increase coronary flow, reduce myocardial oxygen consumption, cerebral blood flow increasing amount, improve soft brain microcirculation and effects such as fluidised form, the chronic microcirculation disturbance of conditioning cardio-cerebrovascular; Blood system there is the anticoagulant effect; Cental system there is sedation; Also have effects such as anti-radiation.Safflower yellow and flavonoid composition have effects such as slight excited heart, increase arteria coronaria and myocardial nutrition property blood flow, anti-experimental character myocardial ischemia, microcirculation improvement to cardiovascular system; Blood system there are anticoagulant and fortifying fibre protein dissolution ability; But also blood fat reducing improves anoxia endurance etc.Radix Puerariae total flavones and Radix Puerariae have effects such as tangible coronary artery dilating, resisting myocardial ischemia and arrhythmia, anticoagulant, blood pressure lowering, blood sugar lowering.Fructus Crataegi has effects such as increasing myocardial contraction and cardiac output, blood pressure lowering, blood fat reducing to cardiovascular system.
At present each medicine is all or part of in each preparation of NAODESHENG is used as medicine with the crude drug powder, and it is too many to extract impurity, and the dosage form of processing also can exist drug effect relatively low, and taking dose is bigger, and then increases patient's burden, and onset waits deficiency slowly.Do not meet the requirement of the modernization of Chinese medicine, be unfavorable for the development of Chinese medicine, influence the research of Chinese medicine compound new drug and move towards international process.
Summary of the invention
The objective of the invention is to deficiency, provide that a kind of impurity is few, the purification process of the active ingredients of compound Naodesheng of good drug efficacy according to prior art.
The object of the invention is achieved through following technical scheme:
A kind of purification process of active ingredients of compound Naodesheng comprises the steps:
(1) the compound Naodesheng raw material is divided into two parts according to the mass fraction, first is Radix Notoginseng 78, Radix Puerariae 261, Fructus Crataegi 157 and Rhizoma Chuanxiong 78; Second portion is a Flos Carthami 91;
(2) in first, add ethanol extraction, after sucking filtration concentrates, obtain the concentrated solution of first; Second portion is used water extraction, behind water-bath, sucking filtration, obtains Flos Carthami extract;
(3) above-mentioned two parts are crossed polyamide respectively and macroporous adsorbent resin adsorbs, eluting, separation and purification;
(4) collect two parts eluent, merge, water-bath concentrates, the evacuation drying under reduced pressure obtains the dry extract of NAODESHENG effective ingredient.
As a kind of preferred version, above-mentioned purification process comprises the steps:
(1) the compound Naodesheng raw material is divided into two parts according to the mass fraction, first is Radix Notoginseng 78, Radix Puerariae 261, Fructus Crataegi 157 and Rhizoma Chuanxiong 78; Second portion is a Flos Carthami 91;
(2) in first, add the ethanol extraction 1～4 time of 4～20 times of quality, every at a distance from 30～90min once, with sucking filtration, merge extractive liquid,, concentrated after, obtain the concentrated solution of first; The water that adds 6～20 times of quality in the second portion, 40～80 ℃ of water-baths 2～3 times, every at a distance from 20～40min once, sucking filtration, merge extractive liquid, obtain Flos Carthami extract;
(3) first's concentrated solution adds water and is settled to the aqueous solution that contains 0.09～0.11g/ml crude drug amount, obtains first's extract; The second portion Flos Carthami extract is settled to the solution that contains 0.06～0.08g/ml crude drug amount through concentrating under reduced pressure, obtains Flos Carthami extract;
(4) above-mentioned two parts extract is crossed polyamide and macroporous adsorbent resin respectively and carry out absorb-elute; The absorb-elute condition that first's extract is crossed resin is: appearance medicinal liquid pH to 1～10 on the accent; Flow velocity absorption with 0.2～5ml/min; Elution flow rate is 1～10ml/min, and the washing volume is 2～10 times of resin column volumes, and it is 10～95wt% that eluting uses concentration of ethanol; The absorb-elute condition that the second portion Flos Carthami extract is crossed resin is: appearance medicinal liquid pH to 1～10 on the accent; Flow velocity absorption with 0.2～10ml/min; Elution flow rate is 1～8ml/min, and the washing volume is 2～10 times of resin column volumes, and it is 10～95wt% that eluting uses concentration of ethanol;
(5) collect two parts ethanol elution, merge, decompression recycling ethanol, 30～90 ℃ of water-baths concentrate, and the evacuation drying under reduced pressure obtains the dry extract of NAODESHENG effective ingredient.
In the above-mentioned steps (2), be preferably in first the concentration that adds 10 times of quality and be the ethanol water-bath reflux, extract, 2 times of 70wt%, every at a distance from 60min once, through sucking filtration, merge extractive liquid,, concentrate after, obtain the concentrated solution of first; The water that adds 14 times of quality in the second portion is in 60 ℃ of water-bath warm macerating 2 times, every at a distance from 30min once, sucking filtration, merge extractive liquid, obtain Flos Carthami extract.
In the above-mentioned steps (4), first preferably carries out adsorption and purification with AB-8, HP20, D101 or D4020 macroporous adsorbent resin, and the Flos Carthami part is preferably carried out adsorption and purification with HPD-100, HP20, D101 or AB-8 macroporous adsorbent resin.Wherein, the absorb-elute condition optimization of first's extract is: appearance medicinal liquid pH to 2～5 on the accent, and with the absorption of 1ml/min flow velocity, elution flow rate is 2～3ml/min, and the washing volume is 4 times of resin column volumes, and the concentration of alcohol that eluting uses is 70wt%; Second portion Flos Carthami extract absorb-elute condition optimization is: appearance medicinal liquid pH to 1～5 on the accent, and with the absorption of 1ml/min flow velocity, elution flow rate is 2～3ml/min, and the washing volume is 6 times of resin column volumes, and eluting uses concentration of ethanol to be 30wt%.
In the above-mentioned steps (5), preferred 45 ℃ of the temperature of said water-bath.
The present invention is in the screening of purification process; Two parts extract is crossed polyamide (comprising 80～100 orders, 30～60 orders and 14～30 orders), macroporous adsorbent resin (comprising D101, D101B, DM130, HP20, S-8, D4020, NKA-9, HPD-100, AB-8, XDA-1, XDA-5, H-20, H-60 and LSA-40), ion exchange resin (comprising anion and cation), epoxy resin, mylar, natural resin, ketone resin, phenolic resins, decolorizing resin, amino resins etc. respectively carry out absorb-elute, so that filter out best purification resin.
Compared with prior art, the present invention has following beneficial effect:
(1) effective rate of transform of purification process of the present invention is high: the present invention is directed to the medicine effect constitutive property, compound Naodesheng is divided into two parts extracts, can extract the effective ingredient of each component so fully, make the process synthesis extraction rate reached to the highest;
(2) extract effective site purity is high: the present invention is through passing through extract the adsorption and purification of the macroporous adsorbent resin that filters out; Dis-medicinal parts such as a large amount of saccharides and tannin have been removed; And the response rate of effective ingredient is raise, obtain the effective site of the higher compound Naodesheng of purity;
(3) the present invention through concentrating under reduced pressure, is convenient to extracting solution, eluent to control temperature and can be reduced concentration time, has reduced loss of active ingredients in the medicine;
(4) the present invention adopts the evacuation drying under reduced pressure with the effective site thick paste, can obviously shorten the heated time of active component, has reduced the loss of composition; Compare with traditional air dry oven; The dry extract that the evacuation hypobaric drying method obtains is loose, and dried powder is convenient to follow-up processing than stable uniform;
(5) AB-8, HP20, D101, D4020 and the HPD-100 macroporous resin of purification process employing of the present invention carry out separation and purification, and the price of these two kinds of resins is lower, and is safe, reduced the purification cost.
Description of drawings
Fig. 1 is a Flos Carthami washing volume curve.
The specific embodiment
Come further to explain the present invention below in conjunction with embodiment, but embodiment does not do any type of qualification to the present invention.
The extraction process experiment of embodiment 1 first
The use ethanol reflux extraction experimentizes, and adopts L
9(3
4) orthogonal experiment method investigates the technological parameter of factors such as alcohol reflux first's amount of ethanol (multiple of quality of medicinal material), concentration of alcohol, extraction time, extraction time; And adopt ultraviolet visible spectrophotometry that the content of total flavones in the extract and total saponins is measured; Measure the content of puerarin, ferulic acid, ginsenoside Rb1, ginsenoside Rg1 and arasaponin R1 simultaneously with high-efficient liquid phase technique, and compare analysis as index.The result sees table 1～table 6.
Table 1 first extraction process factor level table
Table 2 is measured result's four medicines and is closed and put forward weight and comprehensively compare
Table 3 first extraction process orthogonal experiments
The variance analysis of table 4 first
Orthogonal experiments shows (table 3, table 4): what the influence factor was maximum is concentration of alcohol; Extraction time, extraction time, solubilization dosage do not have obvious influence, can find out its influence size ordering C＞A＞B＞D from intuitive analysis, i.e. extraction time and concentration of alcohol influence is bigger; Solubilization dosage and extraction time influence are less relatively; Drawing first thus, to extract selection process be A3B2C2D2, i.e. 70% alcohol reflux twice of 10 times of amounts, 60min/ time.
But concentration of alcohol is last, and horizontal effect is best, again extraction ratio of effective constituents in the extraction process is had the significance influence, so need this factor of concentration of alcohol is tried again single factor investigation test to determine optimised process.
(2) take by weighing first's two parts of prescriptions ratio medical material, extract: a 10 times of amount 70% ethanol extractions twice, 60min/ time by the technology that (1) screening is good; 10 times of amounts of another part, 80% ethanol extraction twice, 60min/ time.Measure the result and see table 5.
Table 5 alcohol extraction is measured the result and is comprehensively compared
The result can find out that 70% alcohol extraction effect is better than 80% alcohol extraction, and it is high that extraction ratio is wanted.So the last optimum extraction process of confirming is 10 times of amount 70% ethanol extractions twice, 60min/ time.
(3) extraction process demonstration test
Took by weighing three parts of the four Chinese medicine material coarse powder (78 parts of Radix Notoginseng, 261 parts of Radix Puerariaes, 157 parts of Fructus Crataegis, 78 parts of Rhizoma Chuanxiongs) of 20 mesh sieves, carried out demonstration test, demonstration test result such as table 6 according to preferred extraction process.
Table 6 first extracts checking and measures the result
Extraction effect is desirable, is superior to each time of orthogonal design experimental result.
Demonstration test result shows that preferred extraction process stablizes feasible.
The extraction process experiment of embodiment 2 second portions
(1) uses water-bath warm macerating method for distilling to experimentize, adopt L
9(3
4) orthogonal experiment method investigates the technological parameter that the water-bath warm macerating extracts second portion amount of water (multiple of quality of medicinal material), extracts factors such as temperature, warm macerating time, lixiviate number of times; And adopt high-efficient liquid phase technique to measure the content of S-A Hydroxysafflor yellow A, and compare analysis as index.The result sees table 7～9.
Table 7 Flos Carthami extraction process factor level table
Table 8 Flos Carthami extraction process orthogonal experiments
Table 9 variance analysis
Orthogonal experiments shows (table 8, table 9): amount of water, extraction time, extraction temperature all have the significance influence to the extraction ratio of hydroxyl A in the water extraction process of Flos Carthami; Can find out its influence size ordering C＞A＞B from intuitive analysis; Be that the influence of extraction time and amount of water is bigger, it is less relatively to extract temperature and times influence, and the water extraction selection process that draws flos carthami is A2B2C2D2; In sum; Selected only process conditions are: add 14 times of water gagings, 60 ℃ of water-bath warm macerating 2 times, 30min/ time.
(2) extraction process demonstration test
Took by weighing three parts of the second portion flos carthami coarse powder (91 parts) of 20 mesh sieves; Carry out demonstration test according to preferred extraction process; Measure S-A Hydroxysafflor yellow A content, three lot sample article S-A Hydroxysafflor yellow A content (mg/g Flos Carthami) are respectively: 9.2460,9.3895,9.4737, and average 9.3697mg/g; Extraction effect is desirable, is superior to each time of orthogonal design experimental result.
Demonstration test result shows that preferred extraction process stablizes feasible.
The resin purification technological experiment of embodiment 3 firsts
Extracting the extracting solution that obtains with aforementioned preferred extraction conditions tests as follows:
(1) screening of resin
To 26 kinds of resin columns having handled well: polyamide (comprising 80～100 orders, 30～60 orders, 14～30 orders), macroporous adsorbent resin (comprising D101, D101B, DM130, HP20, S-8, D4020, NKA-9, HPD-100, AB-8, XDA-1, XDA-5, H-20, H-60, LSA-40), ion exchange resin (comprising anion and cation), epoxy resin, mylar, natural resin, ketone resin, phenolic resins, decolorizing resin, amino resins etc.; 26 parts of an amount of upper props of first's extracting solution of accurate absorption; Absorption is spent the night; Use distilled water, 70% ethanol elution then successively; Collect the each several part eluent, all parallel processing fully of 26 duplicate samples (going up appearance speed 1ml/min, elution speed 2ml/min).The equal testing index property composition of each eluent; And calculate each eluting rate; The comprehensive grading result can know AB-8 (or HP20, D101, D4020), and type macroporous resin adsorption amount is big, eluting rate is high, so adopt AB-8 type (or HP20, D101, D4020) macroporous resin separation and purification first (is representative with the AB-8 type).Confirm as best purification resin.
(2) the upward investigation of appearance concentration
Get the solution that first's upper prop liquid is made into 5 kinds of variable concentrations (concentration is respectively 0.046,0.092,0.138; 0.184; 0.230g/ml), (1.8cm * 30cm), the control flow velocity carries out dynamic adsorption to get with the amount of volume respectively the AB-8 resin column through carrying out pre-treatment; Fully use distilled water, 70% ethanol elution successively after the absorption, collect commensurability each several part eluent and measure.The last appearance of result concentration is respectively 0.046,0.092,0.138,0.184, and during 0.230g/ml, the comprehensive grading adsorption rate is respectively 94.27%, 97.86%, 96.77%, 94.28%, 92.81%, and the visible appearance concentration that goes up is advisable with 0.092g/ml.Reality all can at 0.090～0.110g/ml.
(3) investigation of absorption flow velocity
Get concentration and be the 4 piece AB-8 resin columns of 0.092g/ml extracting solution through carrying out pre-treatment (1.8cm * 30cm); Respectively with 1,2,3, the flow velocity of 4ml/min carries out dynamic adsorption; Fully use distilled water, 70% ethanol elution successively synchronously after the absorption, collect commensurability each several part eluent and measure.The comprehensive grading adsorption rate is respectively 98.32%, 98.01%, 97.21%, 96.44% as a result, and visible absorption flow velocity is advisable with 1ml/min.
(4) investigation of sample solution pH value
Getting concentration is 5 parts of 0.092g/ml sample liquid (pH value of raw sample liquid is 4); With dilute hydrochloric acid or 1wt%NaOH will wherein the pH value of 4 duplicate samples liquid be adjusted to 2,6,8,10 respectively after; All the flow velocity with 1ml/min carries out dynamic adsorption; Fully use distilled water, 70% ethanol elution successively synchronously after the absorption, collect commensurability each several part eluent and measure.PH value is 2,4,6,8,10 o'clock as a result, and the comprehensive grading adsorption rate is respectively 97.52%, 98.57%, 90.49%, 84.40%, 60.98%.It is thus clear that using the sample liquid pH value is 4 o'clock (raw sample liquid), eluting rate is maximum.
(5) the washing volume confirms
The sample liquid that to get 5 times of resin column volumetric concentrations be 0.092g/ml with the flow velocity of 1ml/min through the AB-8 resin column, fully absorption, distillation washing; Collect water lotion; 1 column volume is a, and effluent reacts with molish constantly and detects, and reaction stops washing when being negative; Collect 4 times of resin column volumes this moment, so confirm that the washing amount is 4 times of resin column volumes.
(6) investigation of eluting solvent
After carrying out dynamic adsorption by above-mentioned determined adsorption conditions, resin column is earlier with 4BV distilled water flush away adsorption component not, more respectively with 10%, 30%; 50%, 70%, 90% ethanol liquid finishes to wash post when being eluted on the resin column no obvious color with flow velocity, collects commensurability eluent; Measure the wherein content of each composition, the eluting rate that calculates through the weight comprehensive grading is respectively 17.38%, 36.59%, and 65.78%; 82.12%, 79.13%, visible 70% ethanol of result is best eluant.
(7) investigation of elution speed
After carrying out dynamic adsorption by above-mentioned determined adsorption conditions, be eluant with commensurability 70% ethanol, elution flow rate is respectively 1,2,3,4ml/min.Collect ethanol elution, measure the wherein content of each index components, the eluting rate that calculates through the weight comprehensive grading is respectively 69.27%, 73.68%, and 66.41%, 67.39%.The result is visible, and when elution flow rate was 2ml/min, elute effect was best.
(8) purifying process confirmatory experiment
Took by weighing three parts of the four Chinese medicine material coarse powder (78 parts of Radix Notoginseng, 261 parts of Radix Puerariaes, 157 parts of Fructus Crataegis, 78 parts of Rhizoma Chuanxiongs) of 20 mesh sieves, and extracted according to preferred extraction process, extracting solution carries out upper prop, absorption and eluting respectively by above-mentioned definite absorption, elution requirement.And collect eluent respectively, measure the content of each composition in the eluent.Purification demonstration test result such as table 10.
Table 10 is measured result's four medicines and is closed and put forward weight and comprehensively compare
The result proves that each the index components eluting rate average out to 80.37% after the AB-8 macroporous resin treatment has good repeatability.
The resin purification technological experiment of embodiment 4 second portions
Extracting the Flos Carthami extract that obtains with aforementioned preferred extraction conditions tests as follows:
(1) screening of resin
To 26 kinds of resin columns having handled well: polyamide (comprising 80～100 orders, 30～60 orders, 14～30 orders), macroporous adsorbent resin (comprising D101, D101B, DM130, HP20, S-8, D4020, NKA-9, HPD-100, AB-8, XDA-1, XDA-5, H-20, H-60, LSA-40), ion exchange resin (comprising anion and cation), epoxy resin, mylar, natural resin, ketone resin, phenolic resins, decolorizing resin, amino resins etc.; 26 parts of an amount of upper props of Flos Carthami extract of accurate absorption; Absorption is spent the night; Use distilled water, 50% ethanol elution then successively; Collect the each several part eluent, all parallel processing fully of 17 duplicate samples (going up appearance speed 1ml/min, elution speed 2ml/min).Each eluent is all used the content of high effective liquid chromatography for measuring S-A Hydroxysafflor yellow A; And calculating eluting rate; The result can know HPD-100 type (or HP20, D101, AB-8), and the macroporous resin adsorption amount is big, eluting rate is high, so adopt S-A Hydroxysafflor yellow A (is representative with the HPD-100 type) in HPD-100 type (or HP20, D101, AB-8) the resin separation purification Flos Carthami.
(2) the upward investigation of appearance concentration
Get the solution that the second portion Flos Carthami extract is made into 5 kinds of variable concentrations and (be respectively 0.025,0.050,0.075; 0.100; 0.125g/ml), (1.8cm * 30cm), the control flow velocity carries out dynamic adsorption to get with the amount of volume respectively the HPD-100 resin column through carrying out pre-treatment; Fully use distilled water, 50% ethanol elution successively after the absorption, collect commensurability each several part eluent and carry out assay.The last appearance of result concentration is respectively 0.025,0.050,0.075,0.100, and during 0.125g/ml, the adsorption rate of S-A Hydroxysafflor yellow A is respectively 82.00%, 82.49%, 84.46%, 82.54%, 81.05%, and the visible appearance concentration that goes up is advisable with 0.075g/ml.Reality all can at 0.060～0.080g/ml.
(3) investigation of absorption flow velocity
Get concentration and be the 4 piece HPD-100 resin columns of 0.075g/ml Flos Carthami sample liquid through carrying out pre-treatment (1.8cm * 30cm); Respectively with 1,2,3, the flow velocity of 4ml/min carries out dynamic adsorption; Fully use distilled water, 50% ethanol elution successively synchronously after the absorption, collect commensurability each several part eluent and carry out assay.The last appearance of result flow velocity is respectively 1,2,3, during 4ml/min, the S-A Hydroxysafflor yellow A adsorption rate is respectively 59.02%, 57.94%, 52.02%, 50.89%.It is thus clear that the absorption flow velocity is advisable with 1ml/min.
(4) investigation of sample solution pH value
Getting concentration is 5 parts of 15.6mg/ml Flos Carthami sample liquid (pH value of raw sample liquid is 3); With dilute hydrochloric acid or 1wt%NaOH will wherein the pH value of 4 duplicate samples liquid be adjusted to 1,5,7,9 respectively after; All the flow velocity with 1ml/min carries out dynamic adsorption; Fully use distilled water, 50wt% ethanol elution successively synchronously after the absorption, collect commensurability each several part eluent and carry out assay.PH value is 1,3,5,7,9 o'clock as a result, and the S-A Hydroxysafflor yellow A eluting rate is respectively 35.41%, 62.33%, 53.87%, 50.45%, 26.40%.It is thus clear that using Flos Carthami sample liquid pH value is 3 o'clock (raw sample liquid), eluting rate is maximum.
(5) the washing volume confirms
Determined adsorption conditions more than pressing is got Flos Carthami sample liquid upper prop, carries out dynamic adsorption, uses water elution, collects water elution liquid by 1 resin volume/part, collects 9 parts altogether.The content of S-A Hydroxysafflor yellow A in measuring every part is abscissa with the elution volume umber, and the content of S-A Hydroxysafflor yellow A is the vertical coordinate mapping; See Fig. 1; Visible from figure as a result, when being eluted to 6～7 times of resin volumes not adsorption component wash basically to the greatest extent, in order to reduce the eluting water; Shorten elution time, therefore selecting 6 times of resin volumes is the eluting water consumption.
(6) investigation of eluting solvent
After carrying out dynamic adsorption by above-mentioned determined adsorption conditions, resin column is earlier with 6 times of resin volume distilled water flush awaies adsorption component not, and more respectively with 10%, 30%, 50%, 70%, 90% ethanol liquid is eluted to not to be had when obviously yellow end and wash post on the resin column.Measure the wherein content of hydroxyl A, the eluting rate that calculates S-A Hydroxysafflor yellow A is respectively 81.70%, 98.98%, 94.10%, 92.60%, 73.70%, and the visible 30wt% ethanol of result is best eluant.
(7) investigation of elution speed
After carrying out dynamic adsorption by above-mentioned determined adsorption conditions, be eluant with commensurability 30% ethanol, elution flow rate is respectively 1,2,3,4ml/min.Collect ethanol elution, measure the wherein content of S-A Hydroxysafflor yellow A, the eluting rate that calculates S-A Hydroxysafflor yellow A is respectively 54.48%, 58.91%, 61.59%, 59.43%.It is thus clear that when elution flow rate was 3ml/min, elute effect was best.
(8) purifying process confirmatory experiment
Took by weighing three parts of the flos carthami coarse powder (91 parts) of 20 mesh sieves, and extracted according to preferred extraction process, extracting solution carries out upper prop, absorption and eluting respectively by above-mentioned definite absorption, elution requirement.And collect eluent respectively, measure the content of the yellow A of hydroxyl Flos Carthami in the eluent.The eluting rate that calculates S-A Hydroxysafflor yellow A is respectively 89.62%, 86.41%, 90.92%.The result proves that the S-A Hydroxysafflor yellow A eluting rate average out to 88.98% after the HPD-100 macroporous resin treatment has good repeatability.
Claims (4)
1. the purification process of an active ingredients of compound Naodesheng is characterized in that said method comprises the steps:
(1) the compound Naodesheng raw material is divided into two parts according to the mass fraction, first is Radix Notoginseng 78, Radix Puerariae 261, Fructus Crataegi 157 and Rhizoma Chuanxiong 78; Second portion is a Flos Carthami 91;
(2) concentration that adds 10 times of quality of first is the ethanol water-bath reflux, extract, 2 times of 70wt%, every at a distance from 60min once, through sucking filtration, merge extractive liquid,, concentrate after, obtain the concentrated solution of first; The water that adds 14 times of quality of Flos Carthami is in 60 ℃ of water-bath warm macerating 2 times, every at a distance from 30min once, sucking filtration, merge extractive liquid, obtain Flos Carthami extract;
(3) first's concentrated solution adds water and is settled to the aqueous solution that contains 0.09～0.11g/ml crude drug amount, obtains first's extract; The second portion Flos Carthami extract is settled to the solution that contains 0.06～0.08g/ml crude drug amount through concentrating under reduced pressure, obtains Flos Carthami extract;
(4) above-mentioned two parts extract is crossed polyamide and macroporous adsorbent resin respectively and carry out absorb-elute; The absorb-elute condition that first's extract is crossed resin is: appearance medicinal liquid pH to 1～10 on the accent; Flow velocity absorption with 0.2～5ml/min; Elution flow rate is 1～10ml/min, and the washing volume is 2～10 times of resin column volumes, and it is 10～95wt% that eluting uses concentration of ethanol; The absorb-elute condition that the second portion Flos Carthami extract is crossed resin is: appearance medicinal liquid pH to 1～10 on the accent; Flow velocity absorption with 0.2～10ml/min; Elution flow rate is 1～8ml/min, and the washing volume is 2～10 times of resin column volumes, and it is 10～95wt% that eluting uses concentration of ethanol;
(5) collect two parts ethanol elution, merge, decompression recycling ethanol, 30～90 ℃ of water-baths concentrate, and the evacuation drying under reduced pressure obtains the dry extract of NAODESHENG effective ingredient;
In the step (4), said first carries out adsorption and purification with the AB-8 macroporous adsorbent resin, and Flos Carthami partly carries out adsorption and purification with the HPD-100 macroporous adsorbent resin.
2. the purification process of active ingredients of compound Naodesheng according to claim 1; It is characterized in that in the step (4); The absorb-elute condition of first's extract is: appearance medicinal liquid pH to 2～5 on the accent, and with the absorption of 1ml/min flow velocity, elution flow rate is 2～3ml/min; The washing volume is 4 times of resin column volumes, and the concentration of alcohol that eluting uses is 70wt%.
3. the purification process of active ingredients of compound Naodesheng according to claim 2; It is characterized in that in the step (4); The absorb-elute condition of Flos Carthami extract is: appearance medicinal liquid pH to 1～5 on the accent, and with the absorption of 1ml/min flow velocity, elution flow rate is 2～3ml/min; The washing volume is 6 times of resin column volumes, and eluting uses concentration of ethanol to be 30wt%.
4. the purification process of active ingredients of compound Naodesheng according to claim 1 is characterized in that in the step (5), the temperature of said water-bath is 45 ℃.
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| 大孔吸附树脂分离纯化红花黄色素的工艺研究;雷玉霞等;《医药导报》;20070630;第26卷(第6期);第656-658页 * |
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