CN101041653B - Method for extracting and enriching saussurea involucrate total flavone - Google Patents

Method for extracting and enriching saussurea involucrate total flavone Download PDF

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CN101041653B
CN101041653B CN2007101027482A CN200710102748A CN101041653B CN 101041653 B CN101041653 B CN 101041653B CN 2007101027482 A CN2007101027482 A CN 2007101027482A CN 200710102748 A CN200710102748 A CN 200710102748A CN 101041653 B CN101041653 B CN 101041653B
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extraction
flavones
saussurea
enriching
ethanol
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CN101041653A (en
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赵文军
张富昌
刘明灯
高林
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention discloses an extracting and enriching method of total flavone of saussurea involucrate, which is characterized by the following: proceeding supercritical CO2 extraction for saussurea involucrate; breaking cell wall in the decompressing course after supercritical extraction; reducing the resistance during mass transfer course; stripping low-polarity evaporating component to penetratealcohol and plant component mutually; improving the extracting quantity by 37-120%.

Description

The method of a kind of extraction and enriching saussurea involucrate total flavone
Technical field
The present invention relates to the method for a kind of extraction and enriching saussurea involucrate total flavone
Background technology
Tradition all is directly to use solvent extraction to the extraction of saussurea involucrata effective constituent, and solvent extraction exists solvent load big, needs repeatedly to extract for a long time, because extraction conditions is limited, can not obtain volatile, easy thermolysis composition, deep layer effective constituent leaches difficulty, and medicinal material is utilized rate variance.
Extracting method to the saussurea involucrata flavones provided by the invention carries out supercritical CO after earlier saussurea involucrata being pulverized 2Extraction obtains wherein volatile, and hot unstable composition, and then uses conventional solvent extraction.Discharge in plant materials through the saussurea involucrata flavone component behind the supercritical extraction is easier, its principle is: the decompression deflation course behind the supercritical extraction exists the effect of gas explosion broken wall, greatly reduces second resistance to mass transfer that goes on foot when extracting; Low polarity volatile constituent remove the process that interpenetrates that helps the second step aqueous ethanolic solution and plant component.Through experiment showed, that the saussurea involucrata similarity condition of crossing through first supercritical processing extracts the high 25%-120% of extracted amount (detection of total flavones) to the extraction yield of saussurea involucrata flavones than saussurea involucrata direct solvent next time.
Supercritical CO in the past 2Be only limited to direct extraction low polarity component in the application aspect the effective ingredients in plant extraction, and in fact because effective constituent polar difference, different with plant material, even the complexity that same composition extracts in different plant materialss also has very big difference, such as the direct supercritical extraction of saussurea involucrata flavones, or the effect of extracting under the entrainment agent situation is all undesirable, the present invention extracted and can extract the saussurea involucrata flavone component efficiently in 2 steps, had widened supercritical technology in the medicinal plant Application in Chemistry.
Summary of the invention
The present invention relates to the method for a kind of extraction and enriching saussurea involucrate total flavone, this method is carried out supercritical CO to saussurea involucrata earlier 2Extraction obtains volatile and hot unstable composition wherein, and then uses conventional solvent extraction.Discharge in plant materials through the saussurea involucrata flavone component behind the supercritical extraction is easier.Principle is: the decompression deflation course behind the supercritical extraction exists the effect of gas explosion broken wall, greatly reduces second resistance to mass transfer that goes on foot when extracting; Low polarity volatile constituent remove the process that interpenetrates that helps the second step aqueous ethanolic solution and plant component.Through experiment showed, that the saussurea involucrata similarity condition of crossing through first supercritical processing extracts the high 25%-120% of extracted amount (detection of total flavones) to the extraction yield of saussurea involucrata flavones than saussurea involucrata direct solvent next time.
The method of a kind of extraction of the present invention and enriching saussurea involucrate total flavone follows these steps to carry out:
A, saussurea involucrata is dry and be crushed to 40-200 order postposition and go in the overcritical extraction kettle uses supercritical CO 2Or CO 2Carry ethanol secretly and carry out pre-treatment, dynamic extraction, control extraction kettle pressure 12-40MPa, extraction temperature 30-65 ℃, separating pressure 4-12MPa, separation temperature 20-60 ℃, the time is to stop after 30-180 minute;
The interior recrement of extraction kettle extracts with conventional solvent method after b, the decompression discharging, extracts through 1-2 aqueous ethanolic solution, and extracting temperature is 25-100 ℃, and extraction time is 30-150min, promptly makes the saussurea involucrata flavones and extracts solution;
C, the saussurea involucrata flavone extractive that obtains is evaporated to alcohol concn is the 0%-15% volume ratio, carries out macroporous adsorptive resins absorption;
D, the macroporous adsorbent resin that will adsorb behind the flavones are used 0%95% ethanol elution successively, collect the 30%-50% elutriant, promptly get the Herba Saussureae Involueratae extract that the flavones solid content is 40-50% after concentrating.
Supercutical fluid is independent CO among the step a 2Or CO 2The ethanol of 70%-95% concentration of carrying under one's arms.
Extracting used solvent among the step b is the aqueous ethanolic solution of 50%-95% mass percent concentration.
The consumption of aqueous ethanolic solution is a 7-30 times of mass ratio of saussurea involucrata recrement weight among the step b, and each extraction time is 1-6 hour.
The saussurea involucrata recrement extracts 1-2 time with aqueous ethanolic solution among the step b, and it is the 0%-15% volume ratio that united extraction liquid is concentrated to alcohol concn, for macroporous adsorptive resins absorption.
Used macroporous adsorbent resin is HPD700 or HPD400 or HPD500 among the step c.
Macroporous adsorbent resin described in the steps d is used the ethanolic soln wash-out of 0-95% successively with the flow velocity of 2-8BV/h.
Macroporous adsorbent resin in the steps d after the absorption is a 0%-15% ethanol water liquid gradient elution with concentration earlier, is the 30%-50% ethanol elution with concentration again, collects the ethanol eluate of 30%-50% concentration, gets 40%-50% Saussurea involucrate general flavone extract after concentrating.
The method of a kind of extraction of the present invention and enriching saussurea involucrate total flavone, the comparison of this method and prior art:
Medicinal material and pre-treatment
Herba Saussureae Involueratae (Saussures involucrate) has another name called the snow lotus, is composite family, and hieracioides belongs to per nnial herb.Slurry exsiccant saussurea involucrata herb is crushed to the 40-200 order, and the supercritical carbon dioxide extraction apparatus of packing into then extracts, and extraction conditions is 20MP, and 45 ℃, 2.5h.Recrement after the extraction extracts total flavones as next step solvent method.
Extraction process of the present invention and with conventional extraction method relatively:
The sample extraction comparison is an index with the total flavones amount of extracting before and after the optimization of extraction using alcohol condition and the supercritical carbon dioxide extraction, orthogonal experiment is investigated extraction liquid alcohol concn (50%, 70%, 95%), extraction temperature (45,65,95 ℃), liquid material are than (10,15,20ml/g), the extraction time (1.5,2.5, the 4.0h) influence of four factors.
Measuring result under the orthogonality condition of two kinds of technologies of table 1
Figure DEST_PATH_GSB00000120987200021
According to the quadrature result: in the method 2 under each condition all ratio method 1 extraction yield to exceed 10.07%-128%, relative extraction yield difference maximum when extracting temperature and be 65 ℃, method 1 and 2 top condition are: 95 ℃, 4 hours, 20 times of liquid material ratios, 70% ethanol.The influence factor size is followed successively by: extract temperature, alcohol concn, liquid material ratio, extraction time.Coupling extraction method (method 2) is at 65 ℃, 95 ℃ of 1.5 hours extraction yield (2.91%) and conventional methods (method 1), 2.5 hours extraction yield (2.98%) suitable.
Optimize the contrast of postcondition and document additive method:
With the condition behind the orthogonal optimization respectively according to method 1, method 2 (the inventive method), and method 3 (direct ultrasonic assisted extraction method, 50 times of amount ethanol liquid supersound extraction 30min, add 40 times of ethanol liquid then and continue ultrasonic 45min) the extraction saussurea involucrata, respectively according to 1.4 total flavoness measured in extracting solution, the results are shown in Table 2 thereafter:
Table 2 is optimized postcondition and supersound extraction comparative result
Know that from table with the total flavones extraction yield be index, it is higher by 25.90% than conventional solvent method extraction yield that the conventional solvent method of overcritical coupling extracts Saussurea involucrate general flavone, higher by 35.21% than ultrasonic secondary solvent law part, and reduce consumption of organic solvent.
The HPLC collection of illustrative plates of different methods and the contrast of combined standard product are pointed out:
Extracting solution under conventional solvent method and the overcritical coupled method top condition is HPLC analyzes, the results are shown in Figure, from finger printing as can be known, the difference of two kinds of method extracts component composition under test conditions is very little.In conjunction with the quadrature analysis result, only there is the difference of content in its main component in overcritical coupled method and the traditional extraction method extracting solution.
The Amberlyst process enrichment of Saussurea involucrate general flavone, purifying
The resin Static Adsorption, the investigation of parsing amount and resin preferred, according to document and resin physical parameter, select Cangzhou, Hebei Bao Si company 5 kinds of resins of HPD series (HPD100A, HPD400, HPD500, HPD600 HPD700) investigates the Static Adsorption amount.Measure various resin 10ml respectively,, be placed on behind the Erlenmeyer flask of packing in 30 ℃ of degree constant temperature vibration casees and fully adsorb 24h with the saussurea involucrata flavones aqueous solution 50ml that known flavones concentration is 5.58mg/ml, filter, filtrate constant volume 250ml volumetric flask is surveyed absorbancy, is scaled flavones concentration.
Fully the resin after the absorption is abundant desorption 24h in 30 ℃ of constant temperature vibrations of ethanol elution case of 95% with 100ml concentration.Filter, weigh, filtrate constant volume 250ml volumetric flask is surveyed absorbancy, is scaled flavones concentration.Concentrate the back and survey solid the weight, data see Table:
Several resins of table 3 are to the Static Adsorption of Saussurea involucrate general flavone, static analytic parameter
The resin model HPD100A HPD400 HPD500 HPD600 HPD700
Theoretical adsorptive capacity (mg/ml) 14.73 21.29 18.74 11.55 20.09
Actual adsorptive capacity (mg/ml) 11.14 18.18 17.81 11.92 19.17
The eluate flavones content 27.72％ 35.57％ 38.31％ 30.42％ 36.10％
The flavones rate of recovery 75.66％ 85.37％ 95.05％ 98.02％ 95.39％
Synthesis resin gram adsorptive capacity, eluate flavones percentage composition, flavones rate of recovery result, it is optimum selecting HPD700, also has HPD400, HPD500 preferably.
The dynamic adsorption of HPD700 macroporous resin, dynamically the parsing behavior is investigated
Get HPD700 resin 10.0g (30.67ml) the dress post (blade diameter length ratio 1.25) after the processing, get sample on the aqueous solution that flavones content is 5.58mg/ml, fixedly the pillar flow velocity is 2BV/h (about 1ml/min), sees through the every 15ml portion of liquid, tests it and consolidates weight; The flavones solid content.Data see Table 4:
Table 4HPD700 macroporous resin is to the dynamic saturated absorption of Saussurea involucrate general flavone
See through column volume 1 2 3 4 5 6 7 8 9 10 11
See through liquid-solid heavy (g) 0.42 0.73 0.47 0.66 0.77 0.71 0.72 0.50 0.89 0.72 0.47
Flavones concentration (mg/ml) 0 0 0 0 0 0 0.08 1.02 2.89 3.51 5.62
According to table 4 as can be known the dynamic saturated extent of adsorption of HPD700 resin be about 7.3BV (15 * 7/30.67), the flavones adsorptive capacity is 19.1mg/ml, and is suitable with dynamic saturated extent of adsorption.
Resin ethanol gradient elution concentration after the absorption is investigated:
With each 100ml of Different concentrations of alcohol solution, flow velocity constant (2BV/h) gradient elution
The dynamic gradient analytic parameter of table 5HPD700 macroporous resin
Alcohol concn 0％ 10％ 30％ 50％ 70％ 95％
Wash-out is heavy admittedly 0.094 0.241 0.446 0.739 0.288 0.094
Flavones weight 29.98 53.323 178.4 350.08 27.06 1.02
Eluate flavones solid content 31.89 8.85 40.00 47.37 9.39 1.08
Effective desorption efficiency (mg/ml) 17.7 5.3 17.8 35.0 2.7 0.1
5 parts of 2.5ml of single wash-out resin (0.8149g) behind the saturated respectively upward sample, use the 50ml water elution earlier, use Different concentrations of alcohol 50ml wash-out then respectively, detect eluate weight and flavones content, the results are shown in Table 6
Table 6HPD700 macroporous resin alcohol is resolved concentration parameter and is investigated
Alcohol concn 0％ 10％ 30％ 50％ 70％ 95％
Wash-out is heavy admittedly 57.5 45 66 154 114 122
Flavones weight 5.65 4.98 29.788 52.614 42.399 45.839
Eluate flavones solid content 9.83 11.07 45.13 34.16 37.19 37.57
Active adsorption rate (mg/g) 6.93 6.10 36.55 64.56 52.34 56.59
The method of a kind of extraction of the present invention and enriching saussurea involucrate total flavone, this method has: (1), supercritical CO 2Treatment condition are gentle, can make volatile easy decomposition composition free of losses in the saussurea involucrata, realize the primary separation to effective ingredients in plant, improve the extraction yield of saussurea involucrata flavones, can obtain volatile oil component, the raw material availability height; (2), widened the application of supercritical technology in effective ingredients in plant extracts, simple to operate, safety does not need the gas explosion tank arrangement, whole process is only used alcohol solvent, and the amount ratio ordinary method reduces; (3), it is more overcritical than separately that this coupled method extracts Saussurea involucrate general flavone, or solvent-extraction process all wants high separately, the total flavones extraction yield is higher more than 25% than ordinary method, the medicinal extract that this method obtains is convenient to enrichment and is concentrated flavones, through after the macroporous resin enrichment, can obtain the flavones solid content and be 45% characteristics such as Herba Saussureae Involueratae extract.
Description of drawings
Fig. 1 optimizes the HPLC collection of illustrative plates of back conventional method extracting solution (method 1) for the present invention
Fig. 2 optimizes the HPLC collection of illustrative plates of back coupled method (method 2) for the present invention
Embodiment
Embodiment 1
Get dried saussurea involucrata herb 100g and be crushed to the supercritical extraction reactor of packing into behind 40 orders, start the supercritical co pump, use supercritical CO 2Carry out pre-treatment, set 30 ℃ of extraction temperature, use earlier a spot of CO 2Drain residual air in the system, the pressure extraction still is 12MP then, 30 ℃ of separating still temperature, and regulating separating still pressure is 4MP, dynamic extraction 30 minutes;
After the decompression discharging in the extraction kettle recrement extracts with conventional solvent method, 50% the ethanolic soln of recrement with 7 times of amounts extracted 1 time at 30 ℃, each 1 hour, merging filtrate after the filtration obtained medicinal extract after filtrate is concentrated and contains flavones 3.15g;
The pre-treatment of macroporous adsorbent resin: HPD type macroporous adsorbent resin is before using, sodium chloride solution with 10% soaked 24 hours, sodium chloride solution with 2 times of amounts washes then, and with 5 times of amount deionized water rinsings, so that remove the sanitas of trace and residual monomeric compound; Behind the resin dress post, use alcohol flushing, a small amount of organism and pore-creating agent that flush away is residual are used deionized water rinsing again; With the flushing of 2% sodium hydroxide solution, remove caustic solubility impurity in the resin then, use deionized water rinsing; With the hydrochloric acid soln flushing of 1M, remove solubility in acid impurity again, extremely near neutral with deionized water rinsing;
To obtain saussurea involucrata ethanol extraction 5g, be dispersed in the 100ml hot water, with the HPD400 macroporous resin that the flow velocity of 1BV/h is handled well by 100ml, use 200ml water, 0% then successively, 10%, 40% aqueous ethanolic solution flushing pillar, monitoring sees through the liquid flavones content, and flavones concentration stops to go up sample greater than 0.01mg/ml, collect the ethanol eluate of 40% concentration, merge concentrating and promptly getting the flavones solid content is 44.7% Herba Saussureae Involueratae extract.
Embodiment 2
Get dried saussurea involucrata herb 100g and be crushed to the supercritical extraction reactor of packing into behind 80 orders, start the supercritical co pump, use supercritical CO 2Folder carries out pre-treatment for ethanol, sets 40 ℃ of extraction temperature, uses earlier a spot of CO 2Drain residual air in the system, the pressure extraction still is 20MP then, 40 ℃ of separating still temperature, and regulating separating still pressure is 6MP, dynamic extraction 60 minutes,
Obtain supercritical co saussurea involucrata extract 2.35g in the extraction kettle after the decompression discharging, recrement behind the supercritical extraction extracts 2 times at 60 ℃ with 70% ethanolic soln of 10 times of amounts, each 2 hours, filter the back merging filtrate, obtain medicinal extract after filtrate concentrates and contain flavones 2.35g; And same batch 100g saussurea involucrata is pulverized the back directly with measuring 95% ethanol 65 ℃ of extractions 6 hours with 7 times, obtains medicinal extract and contains flavones and have only 1.35g;
The pre-treatment of macroporous adsorbent resin: HPD type macroporous adsorbent resin is before using, sodium chloride solution with 10% soaked 24 hours, sodium chloride solution with 2 times of amounts washes then, and with 5 times of amount deionized water rinsings, so that remove the sanitas of trace and residual monomeric compound; Behind the resin dress post, use alcohol flushing, a small amount of organism and pore-creating agent that flush away is residual are used deionized water rinsing again; With the flushing of 2% sodium hydroxide solution, remove caustic solubility impurity in the resin then, use deionized water rinsing; With the hydrochloric acid soln flushing of 1M, remove solubility in acid impurity again, extremely near neutral with deionized water rinsing;
To obtain saussurea involucrata ethanol extraction 5g, be dispersed in the 100ml hot water, with the HPD700 macroporous resin that the flow velocity of 3BV/h is handled well by 100ml, use 200ml water, 0% then successively, 10%, 40% aqueous ethanolic solution flushing pillar, monitoring sees through the liquid flavones content, and flavones concentration stops to go up sample greater than 0.01mg/ml, collect the ethanol eluate of 40% concentration, merge concentrating and promptly getting the flavones solid content is 44.7% Herba Saussureae Involueratae extract.
Embodiment 3
Get dried saussurea involucrata herb 100g and be crushed to the supercritical extraction reactor of packing into behind 100 orders, start the supercritical co pump, use supercritical CO 2Carry out pre-treatment, set 45 ℃ of extraction temperature, use earlier a spot of CO 2Drain residual air in the system, the pressure extraction still is 25MP then, 30 ℃ of separating still temperature, and regulating separating still pressure is 4MP, dynamic extraction 150 minutes;
After the decompression discharging, obtain supercritical co saussurea involucrata extract 2.41g from separating still, the recrement behind the supercritical extraction extracts 2 times at 55 ℃ with the ethanol of 7 times of amounts 70%, and each 3 hours, filter the back merging filtrate, obtain medicinal extract after filtrate concentrates and contain flavones 2.49g; And same batch 100g saussurea involucrata is pulverized the back and directly measures 70% ethanol 55 ℃ of extractions 3 hours with 7 times, obtains medicinal extract and contains flavones and have only 1.95g;
The pre-treatment of macroporous adsorbent resin: HPD type macroporous adsorbent resin is before using, sodium chloride solution with 10% soaked 24 hours, sodium chloride solution with 2 times of amounts washes then, and with 5 times of amount deionized water rinsings, so that remove the sanitas of trace and residual monomeric compound; Behind the resin dress post, use alcohol flushing, a small amount of organism and pore-creating agent that flush away is residual are used deionized water rinsing again; With the flushing of 2% sodium hydroxide solution, remove caustic solubility impurity in the resin then, use deionized water rinsing; With the hydrochloric acid soln flushing of 1M, remove solubility in acid impurity again, extremely near neutral with deionized water rinsing;
To obtain saussurea involucrata ethanol extraction 5g, be dispersed in the 100ml hot water, with the HPD500 macroporous resin that the flow velocity of 4BV/h is handled well by 100ml, use 200ml water, 0% then successively, 10%, 40% aqueous ethanolic solution flushing pillar, monitoring sees through the liquid flavones content, and flavones concentration stops to go up sample greater than 0.01mg/ml, collect the ethanol eluate of 40% concentration, merge concentrating and can getting the flavones solid content is 42.9% Herba Saussureae Involueratae extract.
Embodiment 4
Get dried saussurea involucrata herb 100g and be crushed to the supercritical extraction reactor of packing into behind 120 orders, start the supercritical co pump, use supercritical CO 2Carry ethanol secretly and carry out pre-treatment, set 50 ℃ of extraction temperature, use earlier a spot of CO 2Drain residual air in the system, the pressure extraction still is 35MP then, 50 ℃ of separating still temperature, and regulating separating still pressure is 8MP, dynamic extraction 120 minutes;
After the decompression discharging, obtain supercritical co saussurea involucrata extract 2.51g from separating still, the recrement behind the supercritical extraction extracts 2.5 hours time with the ethanol of 15 times of amounts 80% 1 time at 75 ℃, filter the back merging filtrate, obtain medicinal extract after filtrate concentrates and contain flavones 2.91g; And same batch 100g saussurea involucrata is pulverized the back and directly measures 70% ethanol 65 ℃ of extractions 2.5 hours with 15 times, obtains medicinal extract and contains flavones and have only 1.48g
The pre-treatment of macroporous adsorbent resin: HPD type macroporous adsorbent resin is before using, sodium chloride solution with 10% soaked 24 hours, sodium chloride solution with 2 times of amounts washes then, and with 5 times of amount deionized water rinsings, so that remove the sanitas of trace and residual monomeric compound; Behind the resin dress post, use alcohol flushing, a small amount of organism and pore-creating agent that flush away is residual are used deionized water rinsing again; With the flushing of 2% sodium hydroxide solution, remove caustic solubility impurity in the resin then, use deionized water rinsing; With the hydrochloric acid soln flushing of 1M, remove solubility in acid impurity again, extremely near neutral with deionized water rinsing;
To obtain saussurea involucrata ethanol extraction 5g, be dispersed in the 100ml hot water, with the HPD400 macroporous resin that the flow velocity of 1～5BV/h is handled well by 100ml, use 200ml water, 0% then successively, 10%, 40% aqueous ethanolic solution flushing pillar, monitoring sees through the liquid flavones content, and flavones concentration stops to go up sample greater than 0.01mg/ml, collect the ethanol eluate of 40% concentration, merge concentrating and promptly getting the flavones solid content is 44.7% Herba Saussureae Involueratae extract.
Embodiment 5
Getting dried saussurea involucrata herb 100g and be crushed to the supercritical extraction reactor of packing into behind 150 orders, start the supercritical co pump, is that entrainment agent carries out pre-treatment with 95% ethanol, sets 60 ℃ of extraction temperature, uses a spot of CO earlier 2Drain residual air in the system, the pressure extraction still is 35MP then, 50 ℃ of separating still temperature, and regulating separating still pressure is 10MP, dynamic extraction 150 minutes;
After the decompression discharging, obtain supercritical co saussurea involucrata extract 3.52g from separating still, the recrement behind the supercritical extraction extracts 2 times at 85 ℃ with the ethanol of 20 times of amounts 95%, and each 5 hours, filter the back merging filtrate, obtain medicinal extract after filtrate concentrates and contain flavones 2.33g; And same batch 100g saussurea involucrata is pulverized the back and directly measures 95% ethanol 85 ℃ of extractions 5 hours with 7 times, obtains medicinal extract and contains flavones and have only 1.02g;
The pre-treatment of macroporous adsorbent resin: HPD type macroporous adsorbent resin is before using, sodium chloride solution with 10% soaked 24 hours, sodium chloride solution with 2 times of amounts washes then, and with 5 times of amount deionized water rinsings, so that remove the sanitas of trace and residual monomeric compound; Behind the resin dress post, use alcohol flushing, a small amount of organism and pore-creating agent that flush away is residual are used deionized water rinsing again; With the flushing of 2% sodium hydroxide solution, remove caustic solubility impurity in the resin then, use deionized water rinsing; With the hydrochloric acid soln flushing of 1M, remove solubility in acid impurity again, extremely near neutral with deionized water rinsing;
To obtain saussurea involucrata ethanol extraction 5g, be dispersed in the 100ml hot water, with the HPD700 macroporous resin that the flow velocity of 1～5BV/h is handled well by 100ml, use 200ml water, 0% then successively, 10%, 40% aqueous ethanolic solution flushing pillar, monitoring sees through the liquid flavones content, and flavones concentration stops to go up sample greater than 0.01mg/ml, collect the ethanol eluate of 40% concentration, concentrating and can getting the flavones solid content is 45.3% Herba Saussureae Involueratae extract.
Embodiment 6
Get dried saussurea involucrata herb 100g and be crushed to the supercritical extraction reactor of packing into behind 200 orders, start the supercritical co pump, use supercritical CO 2Carry out pre-treatment, set 65 ℃ of extraction temperature, use earlier a spot of CO 2Drain residual air in the system, the pressure extraction still is 40MP then, 60 ℃ of separating still temperature, and regulating separating still pressure is 12MP, dynamic extraction 180 minutes;
After the decompression discharging, obtain supercritical co saussurea involucrata extract 2.35g from separating still, the recrement behind the supercritical extraction extracts 4 hours time with the ethanol of 30 times of amounts 95% 1 time at 100 ℃, filter the back merging filtrate, obtain medicinal extract after filtrate concentrates and contain flavones 3.18g; And same batch 100g saussurea involucrata is pulverized the back and directly measures 95% ethanol 100 ℃ of extractions 4 hours with 30 times, obtains medicinal extract and contains flavones and have only 2.32g;
The pre-treatment of macroporous adsorbent resin: HPD type macroporous adsorbent resin is before using, sodium chloride solution with 10% soaked 24 hours, sodium chloride solution with 2 times of amounts washes then, and with 5 times of amount deionized water rinsings, so that remove the sanitas of trace and residual monomeric compound; Behind the resin dress post, use alcohol flushing, a small amount of organism and pore-creating agent that flush away is residual are used deionized water rinsing again; With the flushing of 2% sodium hydroxide solution, remove caustic solubility impurity in the resin then, use deionized water rinsing; With the hydrochloric acid soln flushing of 1M, remove solubility in acid impurity again, extremely near neutral with deionized water rinsing;
To obtain saussurea involucrata ethanol extraction 5g, be dispersed in the 100ml hot water, with the HPD400 macroporous resin that the flow velocity of 1～5BV/h is handled well by 100ml, use 200ml water, 0% then successively, 10%, 40% aqueous ethanolic solution flushing pillar, monitoring sees through the liquid flavones content, and flavones concentration stops to go up sample greater than 0.01mg/ml, collect the ethanol eluate of 40% concentration, merge concentrating and promptly getting the flavones solid content is 44.7% Herba Saussureae Involueratae extract.

Claims (7)

1. the method for extraction and enriching saussurea involucrate total flavone is characterized in that following these steps to carrying out:
A, saussurea involucrata is dry and be crushed to 40-200 order postposition and go in the overcritical extraction kettle uses supercritical CO 2Or CO 2Carry ethanol secretly and carry out pre-treatment, dynamic extraction, control extraction kettle pressure 12-40MPa, extraction temperature 30-65 ℃, separating pressure 4-12MPa, separation temperature 20-60 ℃, the time is to stop after 30-180 minute;
The interior recrement of extraction kettle extracts with conventional solvent method after b, the decompression discharging, and recrement is extracted through 1-2 aqueous ethanolic solution, and extracting temperature is 25-100 ℃, and extraction time is 30-150min, promptly makes the saussurea involucrata flavones and extracts solution;
C, the saussurea involucrata flavone extractive that obtains is evaporated to alcohol concn is the 0%-15% volume ratio, carries out macroporous adsorptive resins absorption;
D, the macroporous adsorbent resin that will adsorb behind the flavones are used the 0%-95% ethanol elution successively, collect the 30%-50% elutriant, promptly get the Herba Saussureae Involueratae extract that the flavones solid content is 40-50% after concentrating.
2. the method for a kind of extraction according to claim 1 and enriching saussurea involucrate total flavone is characterized in that supercutical fluid is independent CO among the step a 2Or CO 2The ethanol of 70%-95% concentration of carrying under one's arms.
3. the method for a kind of extraction according to claim 1 and enriching saussurea involucrate total flavone is characterized in that extracting used solvent among the step b is the aqueous ethanolic solution of 50%-95% mass percent concentration.
4. according to the method for claim 1 or 3 described a kind of extractions and enriching saussurea involucrate total flavone, the consumption that it is characterized in that aqueous ethanolic solution among the step b is a 7-30 times of mass ratio of saussurea involucrata recrement weight, and each extraction time is 1-6 hour.
5. the method for a kind of extraction according to claim 1 and enriching saussurea involucrate total flavone is characterized in that macroporous adsorbent resin used among the step c is HPD700 or HPD400 or HPD500.
6. a kind of method of extracting with enriching saussurea involucrate total flavone according to claim 1 is characterized in that macroporous adsorbent resin described in the steps d is successively with the flow velocity of the 2-8BV/h ethanolic soln wash-out with 0-95%.
7. the method for a kind of extraction according to claim 1 and enriching saussurea involucrate total flavone, it is characterized in that the macroporous adsorbent resin after the absorption is a 0%-15% ethanol water liquid gradient elution with concentration earlier in the steps d, be the 30%-50% ethanol elution with concentration again, collect the ethanol eluate of 30%-50% concentration, get 40%-50% Saussurea involucrate general flavone extract after concentrating.
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CN102091111B (en) * 2007-12-25 2012-11-21 新疆维吾尔自治区药物研究所 Saussurea cataplasm and production method thereof
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CN108310032A (en) * 2018-03-10 2018-07-24 桐乡市博奥生物科技有限公司 Method based on the extraction of saussurea involucrata callus, enrichment and purifying Saussurea involucrate general flavone
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CN116712474A (en) * 2023-06-20 2023-09-08 齐鲁理工学院 Method for extracting flavonoid substances from herba Saussureae Involueratae by using ultrasonic wave

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