CN104418931A - Extraction condition optimization method and extraction method of tripterygium multi-index active ingredients - Google Patents

Extraction condition optimization method and extraction method of tripterygium multi-index active ingredients Download PDF

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CN104418931A
CN104418931A CN201310379726.6A CN201310379726A CN104418931A CN 104418931 A CN104418931 A CN 104418931A CN 201310379726 A CN201310379726 A CN 201310379726A CN 104418931 A CN104418931 A CN 104418931A
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extraction
ethyl acetate
trypterygine
activeconstituents
liquid ratio
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肖红斌
卓荣杰
张晓哲
王莉
高明哲
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Dalian Institute of Chemical Physics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07J—STEROIDS
    • C07J75/00—Processes for the preparation of steroids in general
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07J—STEROIDS
    • C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
    • C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07J—STEROIDS
    • C07J73/00—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms
    • C07J73/001—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms by one hetero atom
    • C07J73/003—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms by one hetero atom by oxygen as hetero atom
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to an extraction condition optimization method and an extraction method of tripterygium multi-index active ingredients. The extraction condition optimization method is characterized in that against optimal extraction of the tripterygium multi-index active ingredients, an ultrasonic extraction process of the tripterygium active ingredients in the prior art is integrated, through single-factor experimental investigation, three factors, namely liquid-to-solid ratio, solvent concentration and ultrasonic power, which have relatively great effects on extraction overall desirability value (OD value) of the tripterygium multi-index active ingredients, are selected, design expert software is utilized, and a star point design-response surface optimization method is applied for optimization, so that optimal extraction process parameters are obtained. The methods provided by the invention are simple, the experimental precision is high, the optimal values are calculated by model fitting, resources and energy consumption are saved, and a guide can be provided for industrialized extraction and production.

Description

The optimization for extracting condition method of trypterygine multi objective activeconstituents and extracting method
Technical field
The present invention relates to a kind of optimization for extracting condition method of trypterygine multi objective activeconstituents and the extracting method of active ingredients of thunder god vine.
Background technology
Trypterygine has long use history on tcm clinical practice, is mainly used in treating various immunity and diseases associated with inflammation, comprises rheumatoid arthritis, systemic lupus erythematous etc.Active ingredients of thunder god vine has well antitumor, immunosuppression, anti-inflammatory, antifertility, desinsection isoreactivity.Triptolide (i.e. triptolide) is most study in trypterygine, active best composition, has well antitumor, immunosuppression, anti-inflammatory, antifertility, desinsection isoreactivity.Triptonide and triptolide structural similitude, activity is also suitable.Tripterine has very strong antitumor and good immunosuppression isoreactivity.TZ-93 has stronger immunosuppressive action.Therefore these four index activeconstituentss can reflect the overall activity of trypterygine.The domestic and international research to these activeconstituentss at present becomes focus, mainly concentrates on the research and development being carried out original new drug by structure of modification etc., and therefore these active ingredients of thunder god vine of extraction and isolation are significant.
The traditional extracting method of trypterygine has decocting method, circumfluence method, pickling process, percolation.Some new extraction methods, as ultrasonic extraction, supercritical extraction and Smashing extraction method etc., also more and more receive publicity in recent years.But in existing Extraction Technology of Tripterygium, generally only select single index components, the entirety composition of extract can not be weighed; Also have some to the element of the first species as the extraction of total lactones, total alkaloids is reported, but extraction target lacks specific aim, extraction liquid impurity is many; General little employing optimum experimental design, thus cannot judge that whether extraction process is as optimum, whether scientific and reasonable.
Star point design is on the basis of Factorial Design, the experimental design method of the linear or nonlinear fitting of the carrying out formed by factorial point and central point, has that experiment number is few, precision high.Response phase method is according to the regression relation between several variable and one or more dependent variable, the regression relation of extraction conditions and result is obtained by regression analysis, thus try to achieve a kind of Mathematics Optimization Method of optimum extraction process, have science intuitively, the feature such as easily and effectively.
Ultrasonic wave extraction utilizes hyperacoustic cavatition and ultrasonic wave second-order effect to make effective ingredients in plant Fast Stripping, have extract simple and easy, efficiency is high, energy consumption is low, do not destroy the features such as effective constituent.
Summary of the invention
A kind of ultrasonic extraction process using Star point design-response phase method to optimize trypterygine multi objective activeconstituents is the invention provides in order to solve the problem, choose the OD value impact larger factor of liquid ratio, solvent strength and ultrasonic power three on trypterygine multi objective activeconstituents to be optimized, obtain optimum extraction process parameter.
The present invention relates to a kind of optimization for extracting condition method of trypterygine multi objective activeconstituents, it is characterized in that:
1. for the optimized extraction of trypterygine multi objective activeconstituents, extract the trypterygine multi objective activeconstituents optimized can for more than two or three composition in triptolide, Triptonide, Tripterine and TZ-93.
2. use Star point design-response surface optimization method to optimize the ultrasonic extraction process of trypterygine multi objective activeconstituents, carry out according to the following steps:
1) ultrasonic extraction process of comprehensive active ingredients of thunder god vine of the prior art is: the powder getting tripterygium wilfordii root, one or more composition mixing solutionss in methyl alcohol, ethyl acetate, acetonitrile are adopted to extract, according to extraction solution and powder be the liquid ratio of 1:1 ~ 80:1, supersound extraction 5 ~ 60 minutes under 50 ~ 400W power; Solid-liquid separation, must contain the extracting solution of active ingredients of thunder god vine;
2) single factor experiment exam in extraction process:
When other factor is in more excellent horizontal extent, change a certain factor, such as:
When Extraction solvent is ethyl acetate methanol mixing solutions, liquid ratio is at 16:1 ~ 48:1, ultrasonic power is at 100 ~ 400W, extraction time was when the more excellent horizontal extent of 15 ~ 45 minutes, in ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration disperses to choose more than 5 or 6 point values as experimental level in 0 ~ 100% scope, carries out experiment of single factor;
When Extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 50 ~ 100%, ultrasonic power is at 100 ~ 400W, extraction time was when the more excellent horizontal extent of 15 ~ 45 minutes, liquid ratio disperses to choose more than 8 or 9 experimental levels within the scope of 1:1 ~ 80:1, carries out experiment of single factor;
When Extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 50 ~ 100%, liquid ratio is at 16:1 ~ 48:1, extraction time was when the more excellent horizontal extent of 15 ~ 45 minutes, ultrasonic power disperses to choose more than 5 or 6 experimental levels within the scope of 50 ~ 400W, carries out experiment of single factor;
When Extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 50 ~ 100%, liquid ratio is at 16:1 ~ 48:1, ultrasonic power is when the more excellent horizontal extent of 100 ~ 400W, extraction time disperseed to choose more than 6 or 7 experimental levels within the scope of 5 ~ 60 minutes, carried out experiment of single factor;
Empirically solid-liquid separation after supersound extraction, must contain the extracting solution of active ingredients of thunder god vine; Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film; Calculate OD value, OD value is higher, shows that extraction yield is higher, and corresponding Extraction technique is more excellent; Carry out Data Analysis Services (as Fig. 2);
Each process more than in triplicate or four times; Learn according to experiment of single factor examination result, the better parameter of ultrasonic extraction process optimization of trypterygine multi objective activeconstituents is: employing ethyl acetate volumetric concentration is ethyl acetate or the extraction of ethyl acetate methanol mixing solutions of 50 ~ 100%, according to extraction solution and powder be the liquid ratio of 24:1 ~ 40:1, supersound extraction 30 minutes under 100 ~ 400W power;
3) through experiment of single factor examination result, choose liquid ratio, solvent strength and ultrasonic power three affect larger factor to the OD value of trypterygine multi objective activeconstituents, utilize design expert software, use Star point design-response phase method (Li Dongdong, put luxuriant good, high clouds, Deng. Star point design-response phase method optimizes supersound extraction Herbs of Drug Ivyarum polyphenol [J]. Chinese medicinal materials, 2011, 34 (1): 129-133.) be optimized, obtain optimum extraction process parameter: liquid ratio is 34.60, ethyl acetate volumetric concentration is 74.36%, ultrasonic power is 299.5W, supersound extraction 30 minutes.
The invention still further relates to a kind of extracting method of active ingredients of thunder god vine, it is characterized in that: the powder getting tripterygium wilfordii root, employing ethyl acetate volumetric concentration is ethyl acetate or the extraction of ethyl acetate methanol mixing solutions of 50 ~ 100%, according to extraction solution and powder be the liquid ratio of 24:1 ~ 40:1, supersound extraction 30 minutes under 100 ~ 400W power; Solid-liquid separation, must contain the extracting solution of trypterygine multi objective activeconstituents.
The powder of tripterygium wilfordii root refers to and is dried to water ratio≤8%(weight content) tripterygium wilfordii root, by component under the sieve of 60 mesh sieves after pulverizing.
The present invention sums up:
1. the present invention selects multi-target ingredient to carry out extraction optimization, the activeconstituents triptolide of existing low levels and Triptonide, there are again activeconstituents Tripterine and the TZ-93 of high-content, extract while taking into account high low levels main active ingredient and optimize, make extract more fully can reflect the overall activity composition of trypterygine.
2. the present invention's application Star point design-response phase method optimizes trypterygine multi objective activeconstituents extraction process, and Star point design more simplifies than orthogonal design, than uniform design more comprehensively, and the few (orthogonal design 5 of its experiment number 3group experiment), experimental precision is high.
3. in certain embodiments, Extraction solvent can not be methyl alcohol, ethyl acetate, acetonitrile or its mixing solutions; Extraction time can be repeatedly.
4. orthogonal design and homogeneous design are the designs based on linear model, and some design table is as orthogonal design L 9(3 4) be not suitable for secondary and above multinomial model, due to the restriction by selected model, the value direction of a certain factor can only be pointed out, but cannot optimum value be tried to achieve.Star point design-response phase method optimization just tries to achieve optimum value by multinomial model matching, scientificlly and effectively obtains optimum extraction process, best OD value and optimum extraction rate.
5. the present invention adopts ultrasonic wave extraction, have extract simple and easy, efficiency is high, energy consumption is low, do not destroy the advantages such as effective constituent.
6. invention increases the utilization ratio of extraction efficiency and trypterygine resource, saved resource and energy consumption, production can be extracted for the industrialization of trypterygine and guidance is provided.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further details.
The extraction ionic current color atlas of four index activeconstituentss in Fig. 1 trypterygine reference substance solution and extract: triptolide (1), Triptonide (1), TZ-93 (3), Tripterine (4);
Fig. 2 be in experiment of single factor different extraction factor to the effect diagram of trypterygine multi objective activeconstituents OD value:
(1) for liquid ratio is to the effect diagram of trypterygine multi objective activeconstituents OD value
(2) for solvent strength is to the effect diagram of trypterygine multi objective activeconstituents OD value
(3) for ultrasonic power is to the effect diagram of trypterygine multi objective activeconstituents OD value
(4) for extraction time is to the effect diagram of trypterygine multi objective activeconstituents OD value;
Fig. 3 is that the response surface that extraction factor affects trypterygine multi objective activeconstituents OD value is three-dimensional, X-Y scheme:
A () upper figure is the response surface three-dimensional plot that liquid ratio and concentration affect OD value
A () figure below is the response surface X-Y scheme that liquid ratio and concentration affect OD value
B () upper figure is the response surface three-dimensional plot that liquid ratio and ultrasonic power affect OD value
B () figure below is the response surface X-Y scheme that liquid ratio and ultrasonic power affect OD value
C () upper figure is the response surface three-dimensional plot that concentration and ultrasonic power affect OD value
C () figure below is the response surface X-Y scheme that concentration ratio and ultrasonic power affect OD value.
Embodiment
Now be described in further details the present invention with accompanying drawing, embodiment is only limitted to the present invention is described in conjunction with the embodiments, but not limitation of the invention.
Embodiment 1
A kind of optimization for extracting condition method of trypterygine multi objective activeconstituents
1. extract experiment
Weigh the powder getting tripterygium wilfordii root in the balance, one or more composition mixing solutionss in methyl alcohol, ethyl acetate, acetonitrile are adopted to extract, according to extraction solution and powder be the liquid ratio of 1:1 ~ 80:1, supersound extraction 5 ~ 60 minutes under 50 ~ 400W power; Solid-liquid separation, must contain the extracting solution of trypterygine multi objective activeconstituents.Namely (R.J.Zhuo is detected for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film, H.B.Xiao et al.Rapid simultaneous quantitative determination ofterpenoids in Tripterygium wilfordii Hook F by ultrahigh-performance liquidchromatography coupled with quadrupole time-of-flight mass spectrometry.Analytical Methods, 2013,5,2046 – 2052).Utilize the powerful separating power of chromatogram and mass spectrographic high resolution highly sensitive, obtain the extraction ionic current color atlas (see figure 1) of four index activeconstituentss of baseline separation, utilize four compounds integrated peak areas calculate extract general comment value (OD value).
OD=(LOG10(A1*V)*LOG10(A2*V)*LOG10(A3*V)*LOG10(A4*V))^(1/4)
A1, A2, A3, A4 represent extraction ionic current color atlas (EIC) integrated peak areas of four index activeconstituents triptolides, Triptonide, Tripterine, TZ-93 respectively, and V is liquid ratio.
Extraction yield=OD/OD always* 100%
Under optimum extraction conditions, the powder of classification supersound extraction tripterygium wilfordii root, until extracting liquid colourless and can't detect in four activeconstituentss any one, calculate by the actual compound detected, obtain the OD value that each time of classification is extracted, it adds and is OD always.
2. experimental design and statistical study
1) single factor experiment exam in extraction process:
When fixed extraction solvent is ethyl acetate methanol mixing solutions, liquid ratio is 32:1, ultrasonic power is 250W, extraction time is when being 30 minutes, get ethyl acetate volumetric concentration in ethyl acetate methanol mixing solutions and be respectively 0,25,50,75,100%, carry out experiment of single factor, investigate solvent strength to the impact of OD value;
When fixed extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 75%, ultrasonic power is 250W, extraction time is when being 30 minutes, get liquid ratio and be respectively 1:1,2:1,4:1,8:1,16:1,32:1,48:1,80:1, carry out experiment of single factor, investigate liquid ratio to the impact of OD value;
When fixed extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 75%, and liquid ratio is 32:1, extraction time is when being 30 minutes, get ultrasonic power be respectively 50,150,250,350,400W, carry out experiment of single factor, investigate ultrasonic power to the impact of OD value;
When fixed extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 75%, and liquid ratio is 32:1, when ultrasonic power is 250W, getting extraction time is respectively 5,10,15,30,45,60 minutes, carries out experiment of single factor, investigates extraction time to the impact of OD value;
Empirically solid-liquid separation after supersound extraction, must contain the extracting solution of active ingredients of thunder god vine; Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film; Calculate OD value, OD value is higher, shows that extraction yield is higher, and corresponding Extraction technique is more excellent; Carry out Data Analysis Services (as Fig. 2);
Each process more than in triplicate or four times; Learn according to experiment of single factor examination result, the better parameter of ultrasonic extraction process optimization of trypterygine multi objective activeconstituents is: employing ethyl acetate volumetric concentration is ethyl acetate or the extraction of ethyl acetate methanol mixing solutions of 50 ~ 100%, according to extraction solution and powder be the liquid ratio of 24:1 ~ 40:1, supersound extraction 30 minutes under 100 ~ 400W power.
2) response phase method design optimization
According to experiment of single factor examination result, choose these three factors of the impact of OD value more significant liquid ratio, solvent strength and ultrasonic power, utilize design expert software according to Star point design principle contrived experiment, carry out the setting of empirical factor and level, setting the results are shown in Table 1.
Table 1 empirical factor and level set
To extract liquid ratio (X1), solvent strength (X2) and ultrasonic power (X3) for independent variable(s), with OD value for response value (Y), experimental program and data results are in table 2.Experimental point 1-14 is factorial point, and 15-20 is zero point.
The experimental design of table 2 asterism and result
3) foundation of model and statistical study
Multiple regression analysis is carried out, the polynary quadratic regression equation between the variable that meets with a response (liquid ratio, solvent strength and ultrasonic power) and response value (OD value) according to the data obtained.
OD=6.509+0.01823*X1-0.003650*X2+0.02803*X3+0.001128*X1*X2-0.01165*X1*X3-0.002144*X2*X3-0.01021*X1 2-0.04677X2 2-0.01889X3 2
Linear relationship significance between each factor and response value, judged by the inspection of F value, P value is less, and the significance of explanatory variable is higher.From analysis of variance table (table 3), the linear relationship between its dependent variable and all independent variable(s) is (R significantly 2=0.9883), the conspicuous level of model is for being less than 0.0001, so this regression variance model is extremely significant.
The methods analyst result of table 3 experimental data
4) interpretation and optimization
Utilize design expert software to carry out plot analysis according to regression equation, obtain response surface and the isogram thereof of regression equation, as shown in Figure 3.
Learn according to model analysis, the ultrasonic extraction process of trypterygine multi objective activeconstituents is optimized optimum parameter and is: liquid ratio is 34.60, and ethyl acetate volumetric concentration is 74.36%, and ultrasonic power is 299.5W, supersound extraction 30 minutes.With this understanding, OD value reaches 6.522, and extraction rate reached is to 97.50%.
Embodiment 2
Take the powder of tripterygium wilfordii root, add by liquid ratio 32 the ethyl acetate methanol solution that ethyl acetate volumetric concentration is 75%, supersound extraction 30 minutes under 250W ultrasonic power, solid-liquid separation, the extracting solution of trypterygine multi objective activeconstituents must be contained.Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film.Calculating OD value is 6.509, and extraction rate reached is to 97.31%.
Embodiment 3
Take the powder of tripterygium wilfordii root, add by liquid ratio 40 the ethyl acetate methanol solution that ethyl acetate volumetric concentration is 75%, supersound extraction 30 minutes under 250W ultrasonic power, solid-liquid separation, the extracting solution of trypterygine multi objective activeconstituents must be contained.Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film.Calculating OD value is 6.513, and extraction rate reached is to 97.37%.
Embodiment 4
Take the powder of tripterygium wilfordii root, the ethyl acetate methanol solution that ethyl acetate volumetric concentration is 60.57% is added by liquid ratio 27.38, supersound extraction 30 minutes under 336.6W ultrasonic power, solid-liquid separation, must contain the extracting solution of trypterygine multi objective activeconstituents.Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film.Calculating OD value is 6.452, and extraction rate reached is to 96.45%.
Embodiment 5
Take the powder of tripterygium wilfordii root, the ethyl acetate methanol solution that ethyl acetate volumetric concentration is 89.43% is added by liquid ratio 36.62, supersound extraction 30 minutes under 163.4W ultrasonic power, solid-liquid separation, must contain the extracting solution of trypterygine multi objective activeconstituents.Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film.Calculating OD value is 6.443, and extraction rate reached is to 96.32%.
Embodiment 6
Take the powder of tripterygium wilfordii root, add by liquid ratio 32 the ethyl acetate methanol solution that ethyl acetate volumetric concentration is 50%, supersound extraction 30 minutes under 250W ultrasonic power, solid-liquid separation, the extracting solution of trypterygine multi objective activeconstituents must be contained.Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film.Calculating OD value is 6.383, and extraction rate reached is to 95.42%.

Claims (5)

1. the optimization for extracting condition method of a trypterygine multi objective activeconstituents, it is characterized in that: for the optimized extraction of trypterygine multi objective activeconstituents, extract the trypterygine multi objective activeconstituents optimized can for more than two or three composition in triptolide, Triptonide, Tripterine and TZ-93;
Carry out according to the following steps:
1) ultrasonic extraction process of comprehensive active ingredients of thunder god vine of the prior art;
2) single factor experiment exam in extraction process;
3) Star point design-response surface optimization method is used to optimize the ultrasonic extraction process of trypterygine multi objective activeconstituents.
2. according to optimization for extracting condition method according to claim 1, it is characterized in that: use Star point design-response surface optimization method to optimize the ultrasonic extraction process of trypterygine multi objective activeconstituents, carry out according to the following steps:
1) ultrasonic extraction process of comprehensive active ingredients of thunder god vine of the prior art is: the powder getting tripterygium wilfordii root, one or more composition mixing solutionss in methyl alcohol, ethyl acetate, acetonitrile are adopted to extract, according to extraction solution and powder be the liquid ratio of 1:1 ~ 80:1, supersound extraction 5 ~ 60 minutes under 50 ~ 400W power; Solid-liquid separation, must contain the extracting solution of active ingredients of thunder god vine;
2) single factor experiment exam in extraction process:
When other factor is in more excellent horizontal extent, change a certain factor, such as:
When Extraction solvent is ethyl acetate methanol mixing solutions, liquid ratio is at 16:1 ~ 48:1, ultrasonic power is at 100 ~ 400W, extraction time was when the more excellent horizontal extent of 15 ~ 45 minutes, in ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration disperses to choose more than 5 or 6 point values as experimental level in 0 ~ 100% scope, carries out experiment of single factor;
When Extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 50 ~ 100%, ultrasonic power is at 100 ~ 400W, extraction time was when the more excellent horizontal extent of 15 ~ 45 minutes, liquid ratio disperses to choose more than 8 or 9 experimental levels within the scope of 1:1 ~ 80:1, carries out experiment of single factor;
When Extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 50 ~ 100%, liquid ratio is at 16:1 ~ 48:1, extraction time was when the more excellent horizontal extent of 15 ~ 45 minutes, ultrasonic power disperses to choose more than 5 or 6 experimental levels within the scope of 50 ~ 400W, carries out experiment of single factor;
When Extraction solvent is ethyl acetate methanol mixing solutions, ethyl acetate volumetric concentration is 50 ~ 100%, liquid ratio is at 16:1 ~ 48:1, ultrasonic power is when the more excellent horizontal extent of 100 ~ 400W, extraction time disperseed to choose more than 6 or 7 experimental levels within the scope of 5 ~ 60 minutes, carried out experiment of single factor;
Empirically solid-liquid separation after supersound extraction, must contain the extracting solution of active ingredients of thunder god vine; Namely detect for Liquid Chromatography-Tandem Mass Spectrometry after extracting liquid filtering film; Calculate the extraction general comment value (OD value) of trypterygine multi objective activeconstituents, OD value is higher, shows that extraction yield is higher, and corresponding Extraction technique is more excellent;
Each process more than in triplicate or four times; Learn according to experiment of single factor examination result, the better parameter of ultrasonic extraction process optimization of trypterygine multi objective activeconstituents is: employing ethyl acetate volumetric concentration is ethyl acetate or the extraction of ethyl acetate methanol mixing solutions of 50 ~ 100%, according to extraction solution and powder be the liquid ratio of 24:1 ~ 40:1, supersound extraction 30 minutes under 100 ~ 400W power;
3) through experiment of single factor examination result, choose liquid ratio, solvent strength and ultrasonic power three affect larger factor to the OD value of trypterygine multi objective activeconstituents, utilize design expert software, use Star point design-response phase method (Li Dongdong, put luxuriant good, high clouds, Deng. Star point design-response phase method optimizes supersound extraction Herbs of Drug Ivyarum polyphenol [J]. Chinese medicinal materials, 2011, 34 (1): 129-133.) be optimized, obtain optimum extraction process parameter: liquid ratio is 34.60, ethyl acetate volumetric concentration is 74.36%, ultrasonic power is 299.5W, supersound extraction 30 minutes.
3. the extracting method of an active ingredients of thunder god vine, it is characterized in that: the powder getting tripterygium wilfordii root, employing ethyl acetate volumetric concentration is ethyl acetate or the extraction of ethyl acetate methanol mixing solutions of 50 ~ 100%, according to extraction solution and powder be the liquid ratio of 24:1 ~ 40:1, supersound extraction 30 minutes under 100 ~ 400W power; Solid-liquid separation, must contain the extracting solution of trypterygine multi objective activeconstituents.
4. in accordance with the method for claim 3, it is characterized in that:
Liquid ratio is 34.60, and ethyl acetate volumetric concentration is 74.36%, and ultrasonic power is 299.5W, supersound extraction 30 minutes.
5. in accordance with the method for claim 3, it is characterized in that:
The powder of tripterygium wilfordii root refers to and is dried to water ratio≤8%(weight content) tripterygium wilfordii root, by component under the sieve of 60 mesh sieves after pulverizing.
CN201310379726.6A 2013-08-27 2013-08-27 Extraction condition optimization method and extraction method of tripterygium multi-index active ingredients Pending CN104418931A (en)

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Application publication date: 20150318