CN105924540A - Method for synchronously extracting anthraquinone and polysaccharide in morinda officinalis - Google Patents
Method for synchronously extracting anthraquinone and polysaccharide in morinda officinalis Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/74—Rubiaceae (Madder family)
- A61K36/746—Morinda
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention belongs to the field of processing of Chinese herbal medicines, and particularly relates to a method for synchronously extracting anthraquinone and polysaccharide in morinda officinalis. According to the invention, morinda officinalis whole-root dry powder is screened with a 80-mesh sieve, then an ethanol solution with volume fraction of 37% is added according to the material-solution ratio of 1g:37ml for extraction, with the extraction temperature of 60 DEG C, and the extraction time of 77min, then synchronously obtaining an extraction solution containing anthraquinone and polysaccharide, and finally carrying out separation and purification to obtain anthraquinone and polysaccharide respectively. In the conditions, the measured highest extraction rate of anthraquinone in morinda officinalis can reach 85%, and the extraction rate of polysaccharide is 70%. The process is relatively high in extraction rate of anthraquinone and polysaccharide in morinda officinalis in synchronous extraction, and can greatly improve the material utilization rate, shorten the extraction time, reduce the extraction cost, and reduce reagent dosage in a large scale, thus realizing environment-friendly and synchronous extraction of effective components.
Description
Technical field
The invention belongs to the manufacture field of Chinese herbal medicine, be specifically related to anthraquinone and the side of polysaccharide in a kind of simultaneous extraction Radix Morindae Officinalis
Method.
Background technology
Radix Morindae Officinalis (Morinda officinalis How), another name Radix Morindae Officinalis, triangle vine, Herba Morindae Parvifoliae etc., perennial for Rubiaceae
Liana, long 3 ~ 13cm, wide 1.5 ~ 5cm, front end is short tapering, base portion obtuse or circle.The dry root of Radix Morindae Officinalis is oblate post
Shape, slightly curved song.Abound with in Fujian, Guangdong, Hainan, the subtropical and tropical zones such as Guangxi.It is born in mountain region to dredge, under thick forest and shrubbery
In, often climb on shrub or trunk, also have and draw writer's kind.Medicinal plants, cures mainly that impotence and seminal emission, cold womb be infertile, menoxenia, few
Abdomen cold type of pain, rheumatic arthralgia, muscles and bones flaccidity are soft.Its chemical composition has anthraquinone analog compound, saccharide, amino acids, trace element etc..Root
Rubiadin, Rubiadin 1-methylether, physcione, 2-hydroxyl methylol anthraquinone, 1-is had containing anthraquinone component
Hydroxyanthraquinone, 1-hydroxy-2-methyl anthraquinone, 1,6-dihydroxy-2,4-dimethoxy anthraquinone, 1,6-dihydroxy-2-methoxyl group anthracene
Quinone, 2-methylanthraquinone, the also composition Han iridoid；Monotropein, four acetyl rubichloric acid .s.Again containing glucose, mannose, β-paddy
Sterol, Palmic acid and vitamin C, nonadecane, 24-ethyl cholesterol.Root bark is containing 23 kinds of elements such as zinc, manganese, ferrum, chromium.
Conventional industrial abstract, is all to extract anthraquinone and polysaccharide respectively from Radix Morindae Officinalis, and such cycle is the longest, material need to
The amount of asking is big, and chemical levels is big, is contrary to the objective of energy-saving and emission-reduction.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that anthraquinone and polysaccharide in a kind of simultaneous extraction Radix Morindae Officinalis
Method.The present invention first extracts anthraquinone and polysaccharide simultaneously, record Radix Morindae Officinalis anthraquinone high extraction reach 85%, Polyose extraction
Rate is 70%, then extracting solution is carried out lock out operation.Technique process after optimization is few, the cycle is short, save material.
For realizing the purpose of the present invention, adopt the following technical scheme that
Anthraquinone and the method for polysaccharide in a kind of simultaneous extraction Radix Morindae Officinalis: after complete for Radix Morindae Officinalis root dry powder is crossed 80 mesh sieves, by solid-liquid ratio
1g:37ml adds the ethanol solution that volume fraction is 37% and extracts, and Extracting temperature is 60 DEG C, extraction time 77min, it is thus achieved that
Containing anthraquinone and the extracting solution of polysaccharide, last separated purification respectively obtains anthraquinone and polysaccharide.
Described isolated and purified for the extracting solution of acquisition is centrifuged 8min with 4500r/min after, add dehydrated alcohol to carrying
Taking volume fraction of ethanol in liquid is 80%, after standing 24h, then is centrifuged 10min, isolated anthracene with 4500r/min under the conditions of 4 DEG C
Quinone solution and polysaccharide precipitation thing；Carry out being evaporated under reduced pressure by anthraquinone solution and be concentrated into the 1/100 of stock solution volume, be cooled to 1-3 DEG C in advance
Postlyophilization also seals preservation；Polysaccharide precipitation thing adds evaporation after a small amount of distilled water dissolves and removes ethanol, freezing after being cooled to 1-3 DEG C in advance
It is dried and seals preservation.
The present invention has the advantage that compared with the prior art
The technique of anthraquinone and polysaccharide in ethanol solution simultaneous extraction Radix Morindae Officinalis is optimized by the present invention, first extracts anthracene simultaneously
Quinone and polysaccharide, record that Radix Morindae Officinalis anthraquinone high extraction reaches 85%, polysaccharide extract rate is 70%, then carries out extracting solution separating behaviour
Make, anthraquinone and polysaccharide can be respectively obtained.Technique process after optimization is few, the cycle is short, and extraction ratio is higher, significantly carries simultaneously
High raw material availability, shorten extraction time, reduce extraction cost.
Accompanying drawing explanation
Fig. 1 Extracting temperature is to anthraquinone and polysaccharide yield influence curve figure；
Fig. 2 extraction time influence curve figure to anthraquinone and polysaccharide yield；
Fig. 3 volumes of aqueous ethanol mark influence curve figure to anthraquinone and polysaccharide yield；
Fig. 4 solid-liquid ratio influence curve figure to anthraquinone and polysaccharide yield.
Detailed description of the invention
For the openest rather than restriction present invention, below in conjunction with example, the present invention is described in further detail.
Single factor experiment
Respectively with Extracting temperature, extraction time, volume fraction of ethanol and solid-liquid ratio as single-factor variable, extraction time is 1 time, carries
Calculate yield after taking, carry out single factor experiment, and test in triplicate.
, Extracting temperature single factor experiment
Accurately weighing Radix Morindae Officinalis full root dry powder 100g, with volume fraction 40% ethanol solution as extracting solution, fixing solid-liquid ratio is 1:35
(g/ml), extraction time is 70 min, and extraction time is 1 time, and carries out 3 times repeating experiment, investigate Extracting temperature be 40 DEG C, 45
DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C on anthraquinone and the impact of polysaccharide extract rate.
Result of the test is as it is shown in figure 1, along with the meltage of the increase of Extracting temperature, anthraquinone and polysaccharide all increases, due to temperature
After degree is more than 60 DEG C, the biological activity of polysaccharide can drastically decline, therefore with 60 DEG C for optimum extraction temperature.
, extraction time single factor experiment
Accurately weighing Radix Morindae Officinalis full root dry powder 100g, with volume fraction 40% ethanol solution as extracting solution, fixing solid-liquid ratio is 1:35
(g/ml), bath temperature 60 DEG C, extraction time is 1 time, and carries out 3 times repeating experiment, investigation extraction time be 40min,
50min, 60min, 70min, 80min, 90min are on anthraquinone and the impact of polysaccharide extract rate.
Result of the test as in figure 2 it is shown, along with the prolongation of extraction time, Radix Morindae Officinalis anthraquinone and polysaccharide are gradually dissolved out, two
Material extraction ratio is the most in rising trend, and fast after dissolution velocity is the slowest, anthraquinone basically reaches maximum, 80min-when 80min
90min is held essentially constant, and polysaccharide extract rate reaches maximum when 70min.In view of commercial production time, Cost Problems,
Therefore optional 70min is as extraction time.
, volumes of aqueous ethanol mark test
Accurately weighing Radix Morindae Officinalis full root dry powder 100g, fixing solid-liquid ratio is 1:35(g/ml), bath temperature 60 DEG C, extraction time
For 70min, extraction time is 1 time, and carries out 3 times repeating experiment, investigate volumes of aqueous ethanol mark be respectively 25%, 30%,
35%, 40%, 45%, 50% time, on anthraquinone and the impact of polysaccharide extract rate.
Result of the test is as it is shown on figure 3, along with volume fraction of ethanol increases, the extracted amount of anthraquinone increases, when ethanol volume integral
Number is to reach maximum when 40%, increases along with volume fraction of ethanol afterwards, and anthraquinone extracted amount reduces.This is because different volumes
The ethanol solution of mark has different polarity, and according to similar compatibility principle, when volume fraction of ethanol is less, polarity is relatively strong, carries
The substance classes taken out is the most, so being less beneficial to the extraction of anthraquinone, when volume fraction of ethanol is bigger, polarity is more weak, alcohol
Solubility impurity and oil-soluble impurities all are dissolved out, and extraction effect is the most undesirable；On the other hand, volume fraction of ethanol is more than
When 40%, the solvability of water-soluble anthraquinone will weaken.So when volume fraction of ethanol is 40%, the extraction ratio of anthraquinone is
Greatly.Because polysaccharide is water-soluble substances, so polysaccharide stripping quantity when volume fraction of ethanol is less is bigger, along with concentration of alcohol
Increase, the stripping quantity of polysaccharide gradually decreases.
, solid-liquid ratio single factor experiment
Accurately weigh Radix Morindae Officinalis full root dry powder 100g, with volume fraction 40% ethanol solution as extracting solution, bath temperature 60 DEG C, carry
The time of taking is 70min, and extraction time is 1 time, and carries out 3 times repeating experiment, investigate extract solid-liquid ratio be 1:25,1:30,1:35,
1:40,1:45,1:50(g/ml), on anthraquinone and the impact of polysaccharide extract rate.
As shown in Figure 4, Radix Morindae Officinalis anthraquinone and polysaccharide are gradually dissolved out result of the test, and dissolution velocity is gradually slowed by,
When solid-liquid ratio is 1:35 g/ml, anthraquinone, polysaccharide extract rate reach maximum.
The optimum extraction conditions that single factor experiment draws is as shown in table 1 below.
The optimum extraction conditions that table 1 single factor experiment draws
5, response surface optimization extraction process
According to Box-Behnken central combination design principle, in conjunction with the result of single factor experiment, selection and withdrawal temperature, carry
Take time, volume fraction of ethanol, the main investigation factor of solid-liquid ratio four, represent with A, B, C, D respectively, with carrying of anthraquinone and polysaccharide
The rate of taking is response value.Experimental factor level is shown in Table 2.
Table 2 experimental factor and level
Experimental design respectively the results are shown in Table 3.
Table 3 combined extraction technology experimental program and experimental result
Use Design Expert software that response value and each factor are carried out multiple regression matching, draw the one of influence factor
The regressive model equation of secondary effect, quadratic effect and repeatedly response surface of effect.
The regressive model equation of anthraquinone extraction ratio is:
Y=+77.01+10.01*A+2.73*B+1.39*C+1.98*D-0.18*A*B-0.55*A*C+0.75*A*D+0.016*B*
C+0.10*B*D+5.265E-003*C*D-1.59*A2-1.54*B2-3.58*C2-1.75*D2；
In formula: Y represents the extraction ratio of anthraquinone；A, B, C, D represent Extracting temperature, extraction time, volume fraction of ethanol and material respectively
Liquor ratio.
The regressive model equation of polysaccharide extract rate is:
Y=+62.37+4.81*A+2.12*B-6.47*C+0.75*D+0.45*A*B-0.59*A*C+0.27*A*D-0.36*B*C+
0.068*B*D-0.14*C*D-1.74*A2-2.14*B2-1.87*C2-2.77*D2；
In formula: Y represents the extraction ratio of polysaccharide；A, B, C, D represent Extracting temperature, extraction time, volume fraction of ethanol and material respectively
Liquor ratio.
The analysis of variance table such as table 4 below of anthraquinone extraction ratio regressive model.
The analysis of variance table of table 4 anthraquinone extraction ratio regressive model
The analysis of variance table of polysaccharide extract rate regressive model such as table 5 below.
The analysis of variance table of table 5 polysaccharide extract rate regressive model
Anthraquinone regression model is carried out variance analysis, and it the results are shown in Table 4, and block mold has reached pole significant level, i.e. P <
0.0001, show that this quadratic equation has pole significance；Model loses intends item P=0.1434, significantly, shows that the party's formula is to reality
Test fitness preferable；Fitting coefficient R after model adjustment2=0.9626 > 0.85, show that this models fitting seed superiority is higher；Model
The coefficient of variation (CV) is 2.91%, and the reproducible of response value is described；Signal to noise ratio is 27.702 > > 4, precision is sufficiently high.Thus table
This model bright and actual experiment fitting degree are good, and error is little, can be analyzed result of the test with this model and predict.
From the coefficient significance test of regression model, first order A, B, D of model and quadratic term A2B2C2D2To bar
The linear effect impact that in halberd sky, anthraquinone extracts is extremely notable, and first order C is notable on the linear effect impact of anthraquinone in Radix Morindae Officinalis；
It is Extracting temperature, extraction time, solid-liquid ratio, volume fraction of ethanol that each factor affects size to anthraquinone extraction ratio.It is indicated above this
Regression model can preferably describe the true relation between each factor and response value, can determine optimum process condition with it.
Polysaccharide regression model is carried out variance analysis, and it the results are shown in Table 5, and block mold has reached pole significant level, i.e. P <
0.0001, show that this quadratic equation has highly significant；Model loses intends item P=0.8183, significantly, shows the party's formula pair
Experimental fit is preferable；Fitting coefficient R after model adjustment2=0.8956 > 0.85, show that this models fitting seed superiority is higher；Mould
Form variation coefficient (CV) is 5.04%, and the reproducible of response value is described；Signal to noise ratio is 14.286 > > 4, precision is sufficiently high.Thus
Showing that this model and actual experiment fitting degree are good, error is little, can be analyzed result of the test with this model and predict.
From the coefficient significance test of regression model, first order A, C of model and quadratic term A2B2C2D2To Radix Morindae Officinalis
The linear effect impact of middle Polyose extraction is extremely notable, and first order B is notable on the linear effect impact of polysaccharide in Radix Morindae Officinalis；Each factor
It is volume fraction of ethanol, Extracting temperature, extraction time, solid-liquid ratio that polysaccharide extract rate affects size.It is indicated above this recurrence mould
Type can preferably describe the true relation between each factor and response value, can determine optimum process condition with it.
Solvent extraction method is the main method extracting active component in traditional method from the natural drug of complicated component.
The experiment of the design uses ethanol solution water-bath combined extracting to cross the anthraquinone in 80 mesh sieve Radix Morindae Officinalis full root dry powder and polysaccharide, through sound
With water-bath Extracting temperature 60 DEG C, extraction time 77min, volume fraction of ethanol 37%, solid-liquid ratio 1:37 after answering surface Analysis to optimize
(g/ml) it is the optimum extraction condition extraction that carries out anthraquinone and polysaccharide, after extraction, is centrifuged, in 4500r/min, the extraction that 8min obtains
Liquid to add dehydrated alcohol to volume fraction of ethanol be 80%, and 4500r/min is centrifuged 10min after standing 24h in 4 DEG C of refrigerators,
Isolated anthraquinone solution and polysaccharide precipitation thing.Carry out being evaporated under reduced pressure by anthraquinone solution and be concentrated into the 1/100 of stock solution volume, in advance
It is cooled to 1-3 DEG C of postlyophilization and seals preservation；Polysaccharide precipitation thing adds evaporation after a small amount of distilled water dissolves and, except ethanol, is cooled to 1-in advance
3 DEG C of postlyophilizations also seal preservation.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modify, all should belong to the covering scope of the present invention.
Claims (2)
1. anthraquinone and the method for polysaccharide in a simultaneous extraction Radix Morindae Officinalis, it is characterised in that: complete for Radix Morindae Officinalis root dry powder is crossed 80 mesh
After sieve, the ethanol solution adding volume fraction 37% by solid-liquid ratio 1g:37ml extracts, and Extracting temperature is 60 DEG C, extraction time
77min, it is thus achieved that containing anthraquinone and the extracting solution of polysaccharide, last separated purification respectively obtains anthraquinone and polysaccharide.
Anthraquinone and the method for polysaccharide in simultaneous extraction Radix Morindae Officinalis the most according to claim 1, it is characterised in that: described divides
After purification is that with 4500r/min, the extracting solution of acquisition is centrifuged 8min, add dehydrated alcohol to ethanol volume integral in extracting solution
Number is 80%, and after standing 24h under the conditions of 4 DEG C, then it is heavy to be centrifuged 10min, isolated anthraquinone solution and polysaccharide with 4500r/min
Shallow lake thing.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108542949A (en) * | 2018-05-08 | 2018-09-18 | 广西大学 | A kind of ultrasound assisted extraction Morinda officinalis anthraquinone analog compound method |
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| CN102030835A (en) * | 2010-11-03 | 2011-04-27 | 北京佗林医药科技有限公司 | Radix Morindae officinalis extract, preparation method and applications thereof |
| WO2012101741A1 (en) * | 2011-01-24 | 2012-08-02 | 株式会社資生堂 | Tie-2 activator, agent for maturation, normalization, or stabilization of blood vessels, lymph vessel stabilizing agent, wrinkle prevention/improvement agent, and edema improvement/prevention agent |
| CN105477126A (en) * | 2015-12-30 | 2016-04-13 | 广东药学院 | Traditional Chinese medicine extract composition used for treating depression and preparation method and application thereof |
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| CN101874839A (en) * | 2009-04-28 | 2010-11-03 | 仇鑫 | Total effective extractive part of morinda officinalis, as well as preparation method and application thereof |
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| WO2012101741A1 (en) * | 2011-01-24 | 2012-08-02 | 株式会社資生堂 | Tie-2 activator, agent for maturation, normalization, or stabilization of blood vessels, lymph vessel stabilizing agent, wrinkle prevention/improvement agent, and edema improvement/prevention agent |
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| CN108542949A (en) * | 2018-05-08 | 2018-09-18 | 广西大学 | A kind of ultrasound assisted extraction Morinda officinalis anthraquinone analog compound method |
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