CN106491668B - Preparation method of white thorn antioxidative active extractive and products thereof and application - Google Patents
Preparation method of white thorn antioxidative active extractive and products thereof and application Download PDFInfo
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Abstract
The present invention relates to preparation methods of a kind of white thorn antioxidative active extractive and products thereof and application, preparation method include the following steps: by white thorn dry fruit and volume fraction for 30%~95% ethanol water with 1g:(5~30) solid-liquid ratio of mL mixes, cold soaking 1h~4h extracts the mixture of white thorn dry fruit and ethanol water；Obtained solution filtering will be extracted, the filtrate being obtained by filtration is concentrated；Product after concentration is dissolved with water, the obtained solution chromatographic column adsorbing separation for being filled with AB-8 macroreticular resin, the mass ratio of product and macroreticular resin is 1:60~1:100；Chromatographic column is eluted with water to ethanol water elution colourless to efflux, being then 10%~80% with the volume fraction of 10~15 times of column volumes, collects ethanol eluate；Ethanol eluate is concentrated and dried, white thorn antioxidative active extractive is obtained.The preparation method of white thorn antioxidative active extractive provided by the invention, can increase the yield of extract, improve the antioxidant activity of white thorn antioxidative active extractive.
Description
Technical field
The present invention relates to antioxidative active extractive technical fields, and in particular to the white thorn antioxidative active extractive of one kind
Preparation method and products thereof and application.
Background technique
White thorn is the general designation of a variety of machakas of zygophyllaceae (Zygophyllaceae) Nitraria (Nitraria), main
Kind is wanted to have Nitraria sibirica (N.sibirica Pall.) and Nitraria tangutorum (N.tangutorum Bobr.) etc., at me
State is mainly grown in desert or the Semi-desert Area on the ground such as the Inner Mongol, Qinghai, Xinjiang, Gansu, not only there is the work checked winds and fixed drifting sand
With, and its medical value and edible value are also very high, and fruit is sweet in flavor, sour, and it is warm-natured, there are strengthening the spleen and stomach, strengthening by means of tonics, menstruation regulating is lived
The effect of blood, stimulating milk secretion, is usually used in treating weakness of the spleen and the stomach, indigestion, and neurasthenia, hypertension is dizzy, the illnesss such as flu.It is modern
The study found that white thorn is rich in flavones and anthocyanin type components, the ether extract of Nitraria sibirica and the second of Nitraria tangutorum
Acetoacetic ester ingredient or ethanol extract have apparent antioxidant activity.More and more researches show that it is anti-oxidant be pre- anti-aging
Important step, common cancer, artery sclerosis, diabetes, cataract, cardiovascular disease, senile dementia, arthritis etc. are a variety of old
Change related disease is considered to related with free radical.White thorn is used as a kind of natural, is preventing and treating these aging correlation diseases
Sick aspect has good development prospect.
It is in the prior art it is anti-oxidant it is white thorn extract preparation method, using high pressure homogenization technique, membrane separation technique and
The method that macroreticular resin isolation technics combines, although can extract to obtain anti-oxidant white thorn extract, extract yield is low,
Only 0.1%~0.5%, the extract antioxidant activity effect being prepared is also not ideal enough.
Summary of the invention
For the defects in the prior art, it is an object of that present invention to provide a kind of preparations of white thorn antioxidative active extractive
Method and products thereof and application improve the antioxidant activity of white thorn antioxidative active extractive to increase the yield of extract.
To achieve the above object, technical solution provided by the invention are as follows:
In a first aspect, including the following steps: the present invention provides a kind of preparation method of white thorn antioxidative active extractive
By white thorn dry fruit and volume fraction for 30%~95% ethanol water with 1g:(5~30) solid-liquid ratio of mL mixes, cold soaking 1h
~4h, then the mixture of the white thorn dry fruit and the ethanol water is extracted；By the solution mistake extracted and obtained
The filtrate being obtained by filtration is concentrated for filter；Product after the concentration is dissolved with water, obtained solution is with being filled with AB-8
The mass ratio of the chromatographic column adsorbing separation of macroreticular resin, the product and the macroreticular resin is 1:60~1:100；By the color
Spectrum column be eluted with water it is colourless to efflux, then with the volume fraction of 10~15 times of column volumes for 10%~80% ethyl alcohol it is water-soluble
Liquid elution, collects ethanol eluate；The ethanol eluate is concentrated and dried, white thorn antioxidative active extractive is obtained.
In further embodiment of the invention, the volume fraction of the ethanol water being used in mixed way is
50%~70%, the solid-liquid ratio is 1g:30mL.
In further embodiment of the invention, the extracting method of the extraction be heated to reflux, ultrasonic extraction, microwave
One or more of extraction and homogenate extraction.
In further embodiment of the invention, the extracting method is homogenate extraction, the extraction of the homogenate extraction
Number is 3~5 times, and each extraction time of the homogenate extraction is 1min~2min.
In further embodiment of the invention, the extracting method is ultrasonic extraction, the ultrasound of the ultrasonic extraction
Temperature is 40 DEG C, ultrasonic time 60min.
In further embodiment of the invention, the time of the adsorbing separation is 10h~14h.
In further embodiment of the invention, the volume fraction 20% for eluting the ethanol water used
~40%.
In further embodiment of the invention, the white thorn dry fruit is Nitraria tangutorum dry fruit or Nitraria sibirica
Dry fruit.
The preparation method of white thorn antioxidative active extractive provided by the invention, is 30% by white thorn dry fruit and volume fraction
~95% ethanol water is mixed, wherein the solid-liquid ratio of white thorn dry fruit raw material and ethanol water is 1g:(5~30)
ML, solid-liquid ratio can be adjusted according to actual needs；Then cold soaking 1h~4h, cold soaking are the permeability for enhancing solvent, simultaneously
It also helps and leaches more products, the time of cold soaking can be regulated and controled according to actual needs；By white thorn dry fruit and ethanol water
The mixture of solution extracts；Obtained solution filtering will be extracted, the filtrate being obtained by filtration is concentrated, obtained concentration liquid level
Medicinal extract；It by the product after concentration, i.e. medicinal extract, is dissolved with water, the obtained solution containing white thorn oxidation-resistant active ingredient loads
There is a chromatographic column adsorbing separation of AB-8 macroreticular resin, the mass ratio of product and macroreticular resin is 1:60~1:100, quality herein
Than the ratio for referring to product (medicinal extract) and macroreticular resin of unused water dissolution, the purpose of adsorbing separation is by white thorn antioxidant activity
Ingredient is separated with other impurities ingredient, and the quality and product of macroreticular resin and the mass ratio of macroreticular resin can be according to reality
It needs to be adjusted；Chromatographic column is eluted with water colourless to efflux, is then with the volume fraction of 10~15 times of column volumes
10%~80% ethanol water elution, the dosage of ethanol water can be adjusted according to actual needs, collect ethanol elution
Liquid；Ethanol eluate is concentrated and dried, white thorn antioxidative active extractive can be obtained.
Using the preparation method of white thorn antioxidative active extractive provided by the invention, the yield of extract can be increased,
Improve the antioxidant activity of white thorn antioxidative active extractive.
Second aspect, the present invention provides what is be prepared according to the preparation method of above-mentioned white thorn antioxidative active extractive
White thorn antioxidative active extractive.
The third aspect, the present invention provides application of the white thorn antioxidative active extractive in oxidation resistant product.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of the white thorn antioxidative active extractive in the embodiment of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 1, the present invention provides a kind of preparation method of white thorn antioxidative active extractive, include the following steps:
S1: by white thorn dry fruit and volume fraction be 30%~95% ethanol water with 1g:(5~30) solid-liquid ratio of mL
Mixing, cold soaking 1h~4h extract the mixture of the white thorn dry fruit and the ethanol water, the extraction of the extraction
Method be heated to reflux, one or more of ultrasonic extraction, Microwave Extraction and homogenate extraction, the extraction time of the homogenate extraction
Number is 3~5 times, and each extraction time of the homogenate extraction is 1min~2min, and the ultrasonic temperature of the ultrasonic extraction is 40
DEG C, ultrasonic time 60min, solid-liquid ratio ranges preferably from 1g:(5~30) mL, this allows for ratio greater than 1g/mL, no
Conducive to the proposition of extract, ratio is less than 1g/30mL, will cause excessive extracting solution, extends the time of filtering and concentration, increases
Workload；The cold soaking time is preferably 1h~4h, this allows for the leaching for being unfavorable for extract less than 1h, may be made greater than 4h
Complicated reaction occurs for leaching liquid, is unfavorable for obtaining extract；
S2: the obtained solution that extracts is filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after the concentration is dissolved with water, the obtained solution chromatographic column for being filled with AB-8 macroreticular resin
The mass ratio of adsorbing separation, the product and the macroreticular resin is 1:60~1:100, and the time of the adsorbing separation is 10h
~14h is eluted with the ethanol water of 10~15 times of column volumes, is activity, the elution efficiency according to the extract afforded
The preferred scope determined with various factors such as recovery rate；Adsorption time is preferably 10h~14h, is to consider that adsorbing separation is
It is no abundant, to influence extract yield and extract activity；
S4: the chromatographic column being eluted with water colourless to efflux, is then with the volume fraction of 10~15 times of column volumes
10%~80% ethanol water elution, collects ethanol eluate；
S5: the ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
The preparation method of white thorn antioxidative active extractive provided by the invention is made into one combined with specific embodiments below
Walk explanation.
Embodiment one
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 30% by 15g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 4 hours, then the mixture of white thorn dry fruit and ethanol water is subjected to ultrasonic extraction, ultrasound temperature
Degree is 40 DEG C, ultrasonic time 60min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Embodiment two
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 50% by 15g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 4 hours, then the mixture of white thorn dry fruit and ethanol water is subjected to ultrasonic extraction, ultrasound temperature
Degree is 40 DEG C, ultrasonic time 60min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Embodiment three
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 15g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 4 hours, then the mixture of white thorn dry fruit and ethanol water is subjected to ultrasonic extraction, ultrasound temperature
Degree is 40 DEG C, ultrasonic time 60min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Example IV
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 95% by 15g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 4 hours, then the mixture of white thorn dry fruit and ethanol water is subjected to ultrasonic extraction, ultrasound temperature
Degree is 40 DEG C, ultrasonic time 60min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
According to the carry out performance survey for the white thorn antioxidative active extractive that above-described embodiment one to example IV is prepared
Fixed, using anti-oxidant measuring method (DPPH method), specific assay method is as follows:
(1) preparation of DPPH (1,1- diphenyl -2- trinitrophenyl-hydrazine) ethanol solution
Precision weighs 4mgDPPH powder, is placed in the volumetric flask of 50ml, adds dehydrated alcohol to scale, is configured to matter
The solution that concentration is 80 μ g/ml is measured, is shaken up, 4 DEG C of refrigerations are protected from light, spare.
(2) preparation of sample to be tested and reference material solution
Precision weighs appropriate sample to be tested and reference substance, is dissolved and is diluted with water or dehydrated alcohol and is made into 5 various concentrations
Solution (IC50 is within this concentration range), 4 DEG C of refrigerations are protected from light, spare.Vitamin C is the reference material of aqueous samples, dimension
Raw element E is the reference material of fat-soluble sample.
(3) anti-oxidant measuring method
By various concentration sample to be tested and reference substance solution, respectively take 100 μ L that the DPPH ethanol solution of 80 μ g/mL is added
100 μ L are covered, shaking, measure absorbance value under 517nm after avoid light place 30min.100 μ L sample solution and 100 μ LDPPH
The mixed liquor of ethanol solution, as measurement group；The mixed liquor of 100 μ L sample solution and 100 μ L dehydrated alcohols, as blank
Group；The mixed liquor of 100 μ L sample solvents and 100 μ LDPPH solution, as a control group.
DPPH clearance rate (%)={ 1- (Asample-Ablamk)/Acontrol } × 100%
Asample: the absorbance value (100 μ L) of the mixed liquor of sample solution (100 μ L)+DPPH solution
Ablank: the absorbance value (100 μ L) of the mixed liquor of sample solution (100 μ L)+dehydrated alcohol
Acontrol: the absorbance value (100 μ L) of the mixed liquor of sample solvent (100 μ L)+DPPH solution
With DPPH clearance rate (%) Y to sample solution mass concentration X, clearance rate curve is drawn, clearance rate and concentration are obtained
Linear equation, then calculate and acquire IC50.
Height is passed through using identical Nitraria sibirica dry fruit raw material to above-described embodiment one to example IV and comparative example
The white thorn antioxidant activity that the method that pressure homogeneous technology, membrane separation technique and macroreticular resin isolation technics combine is prepared mentions
Object is taken to carry out performance measurement, the extract yield being calculated and IC50 result are as shown in table 1 below:
The result (n=3) for the extract that table 1 is obtained using the ethanol water of different volumes score
| Embodiment | Sample | Extract yield | IC50(mg/mL) |
| Embodiment one | 30% ethanol extract | 1.233% | 0.1931 |
| Embodiment two | 50% ethanol extract | 1.875% | 0.0625 |
| Embodiment three | 70% ethanol extract | 2.129% | 0.0427 |
| Example IV | 95% ethanol extract | 1.476% | 0.1784 |
| Comparative example | - | 0.327% | 0.8289 |
Embodiment five
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: the second that the volume fraction by 5g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and 150mL is 70%
Alcohol solution mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction, homogenate extraction
Extraction time be 5 times, each extraction time of homogenate extraction is 1min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Embodiment six
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: the second that the volume fraction by 5g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and 150mL is 70%
Alcohol solution mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to ultrasonic extraction, ultrasonic temperature
It is 40 DEG C, ultrasonic time 60min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Embodiment seven
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: the second that the volume fraction by 5g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and 150mL is 70%
Alcohol solution mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to heating and refluxing extraction, heating
Return time is 1 hour；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Embodiment eight
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: the second that the volume fraction by 5g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2014) and 150mL is 70%
Alcohol solution mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to Microwave Extraction, Microwave Extraction
Time be 30min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water to second colourless to efflux, being then 40% with the volume fraction of 15 times of column volumes
Alcohol solution elution, collects ethanol eluate；
S5: ethanol eluate is concentrated and dried, and obtains white thorn antioxidative active extractive.
Using above-mentioned same performance measurement method, the white thorn antioxygen that above-described embodiment five to embodiment eight is prepared
Change activity extract and carry out performance measurement, the extract yield being calculated and IC50 result are as shown in table 2 below:
The result (n=3) for the extract that table 2 is extracted using different extracting modes
| Embodiment | Extraction process | Extract yield | IC50(mg/mL) |
| Embodiment five | Sudden strain of a muscle mentions | 1.347% | 0.2630 |
| Embodiment six | Ultrasound | 1.579% | 0.2572 |
| Embodiment seven | Reflux | 1.032% | 0.3775 |
| Embodiment eight | Microwave | 0.968% | 0.4653 |
Embodiment nine
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 15g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2015) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction, it is flash to mention
The extraction time taken is 5 times, and homogenate extraction each extraction time is 1min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 10%,
20%, 40%, 80% ethanol water elution, collects ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
Using above-mentioned same performance measurement method, above-described embodiment nine is eluted using the ethanol water of different volumes
The performance of obtained white thorn antioxidative active extractive is measured, and the IC50 result being calculated is as shown in table 3 below:
The result (n=3) for the extract that table 3 is eluted using the ethanol water of different volumes score
| Eluting liquid fraction | Extract yield | IC50(mg/mL) |
| 10% ethanol water | 2.455% | 0.1591 |
| 20% ethanol water | 0.912% | 0.0689 |
| 40% ethanol water | 1.597% | 0.0533 |
| 80% ethanol water | 0.523% | 0.1898 |
Embodiment ten
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: it is by 15g Nitraria sibirica dry fruit (is produced from the Inner Mongol, lot number NMG-2015) and the volume fraction of 450mL
70% ethanol water mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction,
The extraction time of homogenate extraction is 5 times, and each extraction time of homogenate extraction is 1min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 10%,
20%, 40%, 80% ethanol water elution, collects ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
Using above-mentioned same performance measurement method, above-described embodiment ten is eluted using the ethanol water of different volumes
The performance of obtained white thorn antioxidative active extractive is measured, and the IC50 result being calculated is as shown in table 4 below:
The result (n=3) for the extract that table 4 is eluted using the ethanol water of different volumes score
| Eluting liquid fraction | Extract yield | IC50(mg/mL) |
| 10% ethanol water | 3.838% | 0.2208 |
| 20% ethanol water | 1.601% | 0.1014 |
| 40% ethanol water | 8.971% | 0.4860 |
| 80% ethanol water | 2.528% | 0.7050 |
Embodiment 11
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 385g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2015) and the volume fraction of 11550mL
Ethanol water mixing, cold soaking 1 hour, then by it is white thorn dry fruit and ethanol water mixture carry out homogenate extraction, it is flash
The extraction time of extraction is 3 times, and each extraction time of homogenate extraction is 2min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 10%,
40% ethanol water elution, collects ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
Using above-mentioned same performance measurement method, to above-described embodiment 11 using the ethanol aqueous wash of different volumes
The performance of de- obtained white thorn antioxidative active extractive is measured, and the IC50 result being calculated is as shown in table 5 below:
The result (n=3) for the extract that table 5 is eluted using the ethanol water of different volumes score
| Eluting liquid fraction | Extract yield | IC50(mg/mL) |
| 10% ethanol water | 7.267% | 0.248 |
| 40% ethanol water | 3.301% | 0.0485 |
Embodiment 12
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 385g Nitraria sibirica dry fruit (is produced from Qinghai, lot number QH2015) and the volume fraction of 11550mL
Ethanol water mixing, cold soaking 1 hour, then by it is white thorn dry fruit and ethanol water mixture carry out homogenate extraction, it is flash
The extraction time of extraction is 3 times, and each extraction time of homogenate extraction is 2min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 40%
Ethanol water elution, collect ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
It is with the DPPH method measurement as above white antioxidant activity IC50 value for piercing antioxidative active extractive obtained
0.049mg/mL, extractive content 19.97g.
Embodiment 13
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 30g Nitraria sibirica dry fruit (is produced from Xinjiang, lot number XJ2015) and the volume fraction of 900mL
Ethanol water mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction, it is flash to mention
The extraction time taken is 3 times, and homogenate extraction each extraction time is 2min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 40%
Ethanol water elution, collect ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
It is with the DPPH method measurement as above white antioxidant activity IC50 value for piercing antioxidative active extractive obtained
0.052mg/mL, extractive content 0.86g.
Embodiment 14
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 30g Nitraria tangutorum dry fruit (is produced from the Inner Mongol, lot number NMG2015) and the volume fraction of 900mL
Ethanol water mixing, cold soaking 1 hour, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction, it is flash to mention
The extraction time taken is 3 times, and each extraction time of homogenate extraction is 2min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:100, and the time of adsorbing separation is 12h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 20%
Ethanol water elution, collect ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
It is with the DPPH method measurement as above white antioxidant activity IC50 value for piercing antioxidative active extractive obtained
0.10mg/mL, extractive content 0.52g.
Embodiment 15
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 30g Nitraria tangutorum dry fruit (is produced from the Inner Mongol, lot number NMG2015) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 2 hours, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction, it is flash to mention
The extraction time taken is 4 times, and each extraction time of homogenate extraction is 1.5min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:60, and the time of adsorbing separation is 10h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 10 times of column volumes be 40%
Ethanol water elution, collect ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
It is with the DPPH method measurement as above white antioxidant activity IC50 value for piercing antioxidative active extractive obtained
0.097mg/mL, extractive content 0.53g.
Embodiment 16
The preparation method for present embodiments providing a kind of white thorn antioxidative active extractive, includes the following steps:
S1: being 70% by 30g Nitraria tangutorum dry fruit (is produced from the Inner Mongol, lot number NMG2015) and the volume fraction of 450mL
Ethanol water mixing, cold soaking 2 hours, then the mixture of white thorn dry fruit and ethanol water is subjected to homogenate extraction, it is flash to mention
The extraction time taken is 4 times, and each extraction time of homogenate extraction is 1.5min；
S2: obtained solution will be extracted and filtered, the filtrate being obtained by filtration is concentrated, medicinal extract is obtained；
S3: the product after concentration is dissolved with water, the chromatographic column absorption for being filled with AB-8 macroreticular resin of obtained solution
The mass ratio of separation, product and macroreticular resin is 1:80, and the time of adsorbing separation is 14h；
S4: chromatographic column is eluted with water it is colourless to efflux, then respectively with the volume fraction of 13 times of column volumes be 40%
Ethanol water elution, collect ethanol eluate respectively；
S5: ethanol eluate is concentrated and dried respectively, obtains white thorn antioxidative active extractive.
It is with the DPPH method measurement as above white antioxidant activity IC50 value for piercing antioxidative active extractive obtained
0.078mg/mL, extractive content 0.65g.
It is other solid-liquid ratios, cold it should be noted that the case where in addition to selecting above-described embodiment one to embodiment 16 to enumerate
Leaching time, elution ethanol water dosage, adsorption time, white thorn dry fruit type and the place of production be also it is feasible, only implementing
In the case that example one is enumerated to embodiment 16, the activity of extract and the resultant effect of extract yield are more preferable.
The preparation method of white thorn antioxidative active extractive provided by the invention, can increase the yield of extract, improve
The antioxidant activity of white thorn antioxidative active extractive.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant, and it does not separate the essence of the corresponding technical solution various embodiments of the present invention skill
The range of art scheme should all cover within the scope of the claims and the description of the invention.
Claims (3)
1. a kind of preparation method of white thorn antioxidative active extractive, which comprises the steps of:
White thorn dry fruit is mixed with the ethanol water that volume fraction is 50%~70% with the solid-liquid ratio of 1g:30mL, cold soaking 1h
~4h, then the mixture of the white thorn dry fruit and the ethanol water is extracted；The extracting method of the extraction is to add
One or more of hot reflux, ultrasonic extraction, Microwave Extraction and homogenate extraction；When the extracting method is homogenate extraction, institute
The extraction time for stating homogenate extraction is 3~5 times, and each extraction time of the homogenate extraction is 1min~2min；The extraction
When method is ultrasonic extraction, the ultrasonic temperature of the ultrasonic extraction is 40 DEG C, ultrasonic time 60min；The white thorn dry fruit is
Nitraria tangutorum dry fruit or Nitraria sibirica dry fruit；
By the solution filtering extracted and obtained, the filtrate being obtained by filtration is concentrated；
Product after the concentration is dissolved with water, the chromatographic column absorption point for being filled with AB-8 macroreticular resin of obtained solution
From the mass ratio of the product and the macroreticular resin is 1:60~1:100；The time of the adsorbing separation is 10h~14h；
The chromatographic column is eluted with water it is colourless to efflux, then with the volume fraction of 10~15 times of column volumes be 20%~
40% ethanol water elution, collects ethanol eluate；
The ethanol eluate is concentrated and dried, white thorn antioxidative active extractive is obtained.
2. the anti-oxidant work of white thorn that the preparation method of white thorn antioxidative active extractive according to claim 1 is prepared
Property extract.
3. white thorn antioxidative active extractive as claimed in claim 2 is preparing the application in oxidation resistant product.
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| CN106924306A (en) * | 2017-05-17 | 2017-07-07 | 中国科学院新疆理化技术研究所 | A kind of preparation method of Nitraria sibirica fruit general flavone |
| CN110693925A (en) * | 2019-10-10 | 2020-01-17 | 南京益唯森生物科技有限公司 | Ultrasonic-assisted extraction process of Nitraria tangutorum bobr pulp |
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| CN101991641A (en) * | 2010-11-09 | 2011-03-30 | 中国科学院西北高原生物研究所 | Preparation method of antioxidation nitraria tangutorum bobr extractive |
| CN103110674A (en) * | 2013-02-01 | 2013-05-22 | 中国林业科学研究院 | Nitraria tangutorum bobr total phenolic extract, as well as extraction method and application thereof |
| CN105213442A (en) * | 2015-10-28 | 2016-01-06 | 青海尤尼克生物技术有限公司 | A kind of Fructus Nitraria schoberi extractive of general flavone and preparation method thereof |
| CN105232593A (en) * | 2015-10-28 | 2016-01-13 | 青海尤尼克生物技术有限公司 | Nitraria branch and leaf extract |
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| CN101991641A (en) * | 2010-11-09 | 2011-03-30 | 中国科学院西北高原生物研究所 | Preparation method of antioxidation nitraria tangutorum bobr extractive |
| CN103110674A (en) * | 2013-02-01 | 2013-05-22 | 中国林业科学研究院 | Nitraria tangutorum bobr total phenolic extract, as well as extraction method and application thereof |
| CN105213442A (en) * | 2015-10-28 | 2016-01-06 | 青海尤尼克生物技术有限公司 | A kind of Fructus Nitraria schoberi extractive of general flavone and preparation method thereof |
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