CN106491668A - 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 a kind of preparation method and products thereof of white thorn antioxidative active extractive and application, preparation method comprises the steps：By thorn dry fruit in vain with the ethanol water that volume fraction is 30%～95% with 1g:The mixture of thorn dry fruit and ethanol water in vain is extracted by the solid-liquid ratio mixing of (5～30) mL, cold soaking 1h～4h；The solution filtration for obtaining will be extracted, the filtrate being filtrated to get will be concentrated；Products in water dissolving after by concentration, the solution for the obtaining chromatographic column adsorbing separation for being filled with 8 macroreticular resins of AB, product are 1 with the mass ratio of macroreticular resin:60～1:100；Chromatographic column is washed with water colourless to efflux, then the volume fraction with 10～15 times of column volumes be 10%～80% ethanol water wash-out, collect ethanol eluate；By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.The preparation method of the white thorn antioxidative active extractive that the present invention is provided, can increase the yield of extract, improve the antioxidation activity of white thorn antioxidative active extractive.
Description
Technical field
The present invention relates to antioxidative active extractive technical field, and in particular to a kind of white thorn antioxidative active extractive
Preparation method and products thereof and application.
Background technology
White thorn is the general designation of multiple 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 the desert on the ground such as the Inner Mongol, Qinghai, Xinjiang, Gansu or Semi-desert Area, the work that does not only check winds and fix drifting sand
With, and its medical value and edibility are also very high, and fruit is sweet, sour, warm in nature, has strengthening the spleen and stomach, strengthening by means of tonics, menstruation regulating to live
The effect of blood, lactagogue, it is usually used in treating weakness of the spleen and the stomach, indigestion, neurasthenia, hypertension are dizzy, the illness such as flu.Modern
Research finds that white thorn is rich in flavones and anthocyanin type components, the second of the ether extract and Nitraria tangutorum of Nitraria sibirica
Acetoacetic ester composition or ethanol extract have obvious antioxidation activity.Increasing research shows that anti-oxidant is pre- anti-aging
Important step, common cancer, artery sclerosis, diabetes, cataract, cardiovascular disease, senile dementia, arthritis etc. are multiple old
Change relevant disease is considered to relevant with free radical.White thorn is preventing and treating these aging related diseases as a kind of natural
Sick aspect has good DEVELOPMENT PROSPECT.
Of the prior art anti-oxidant 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 and obtain anti-oxidant white thorn extract, but extract yield is low,
Only 0.1%～0.5%, the extract antioxidation activity effect for preparing is also not ideal enough.
Content of the invention
For defect of the prior art, present invention aim at providing a kind of preparation of white thorn antioxidative active extractive
Method and products thereof and application, to increase the yield of extract, improve the antioxidation activity of white thorn antioxidative active extractive.
For achieving the above object, the technical scheme of present invention offer is：
In a first aspect, the invention provides a kind of preparation method of white thorn antioxidative active extractive, comprises the steps：
By thorn dry fruit in vain with the ethanol water that volume fraction is 30%～95% with 1g:The solid-liquid ratio mixing of (5～30) mL, cold soaking 1h
～4h, then the mixture of the white thorn dry fruit and the ethanol water is extracted；By the solution mistake that extracts and obtain
Filter, by the filtrate concentration being filtrated to get；Products in water after the concentration is dissolved, the solution for obtaining is with being filled with AB-8
The chromatographic column adsorbing separation of macroreticular resin, the product are 1 with the mass ratio of the macroreticular resin:60～1:100；By the color
Spectrum post wash with water colourless to efflux, then the volume fraction with 10～15 times of column volumes be 10%～80% ethanol water-soluble
Liquid is eluted, and collects ethanol eluate；By the ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
In the further embodiment of the present invention, the volume fraction of the ethanol water being used in mixed way is
50%～70%, the solid-liquid ratio is 1g:30mL.
In the further embodiment of the present invention, the extracting method of the extraction is for being heated to reflux, ultrasonic extraction, microwave
Extract and one or more in homogenate extraction.
The present invention further embodiment in, the extracting method be homogenate extraction, the extraction of the homogenate extraction
Number of times is 3～5 times, and each extraction time of the homogenate extraction is 1min～2min.
The present invention further embodiment in, the extracting method be ultrasonic extraction, the ultrasound of the ultrasonic extraction
Temperature is 40 DEG C, and ultrasonic time is 60min.
In the further embodiment of the present invention, the time of the adsorbing separation is 10h～14h.
In the further embodiment of the present invention, the volume fraction 20% for eluting the ethanol water for using
～40%.
In the further embodiment of the present invention, the white thorn dry fruit is Nitraria tangutorum dry fruit or Nitraria sibirica
Dry fruit.
The preparation method of the white thorn antioxidative active extractive that the present invention is provided, it is 30% that will pierce dry fruit in vain with volume fraction
～95% ethanol water is mixed, and wherein thorn dry fruit raw material is 1g with the solid-liquid ratio of ethanol water in vain:(5～30)
ML, solid-liquid ratio can be adjusted according to actual needs；Then cold soaking 1h～4h, cold soaking are the permeability for strengthening solvent, while
The more products of leaching are also helped, the time of cold soaking can be regulated and controled according to actual needs；Dry fruit and ethanol water will be pierced in vain will
The mixture of solution is extracted；The solution filtration for obtaining will be extracted, the filtrate being filtrated to get be concentrated, the concentration liquid level for obtaining
Medicinal extract；Product after by concentration, i.e. medicinal extract, with water dissolves, the solution filling containing thorn oxidation-resistant active ingredient in vain for obtaining
There is the chromatographic column adsorbing separation of AB-8 macroreticular resins, product is 1 with the mass ratio of macroreticular resin:60～1:100, quality herein
Than referring to the ratio of unused water-soluble product (medicinal extract) and macroreticular resin, the purpose of adsorbing separation is to be pierced antioxidation activity in vain
Composition is separated with other impurities composition, and the mass ratio of the quality of macroreticular resin and product and macroreticular resin can be according to reality
Needs are adjusted；Chromatographic column is washed with water colourless to efflux, then with the volume fraction of 10～15 times of column volumes be
10%～80% ethanol water wash-out, the consumption of ethanol water can be adjusted according to actual needs, collect ethanol elution
Liquid；By ethanol eluate concentrate drying, you can obtain white thorn antioxidative active extractive.
The preparation method of the white thorn antioxidative active extractive provided using the present invention, can increase the yield of extract,
Improve the antioxidation activity of white thorn antioxidative active extractive.
Second aspect, the invention provides prepared according to the preparation method of above-mentioned white thorn antioxidative active extractive
White thorn antioxidative active extractive.
The third aspect, the invention provides thorn application of the antioxidative active extractive in oxidation resistant product in vain.
The additional aspect and advantage of the present invention will be set forth in part in the description, and partly will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Description of the drawings
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
Accompanying drawing in below in conjunction with the embodiment of the present invention, to the embodiment of the present invention in technical scheme carry out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiment.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
As shown in figure 1, the present invention provides a kind of preparation method of white thorn antioxidative active extractive, comprise the steps：
S1：By thorn dry fruit in vain with the ethanol water that volume fraction is 30%～95% with 1g:The solid-liquid ratio of (5～30) mL
The mixture of the white thorn dry fruit and the ethanol water is extracted, the extraction of the extraction by mixing, cold soaking 1h～4h
Method be heated to reflux, one or more in 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 is 60min, and solid-liquid ratio ranges preferably from 1g:(5～30) mL, this allow for ratio and are more than 1g/mL, no
Beneficial to the proposition of extract, ratio can cause excessive extract less than 1g/30mL, extend the time that filters and concentrate, and increase
Workload；The cold soaking time is preferably 1h～4h, and this allows for the leaching for being unfavorable for extract less than 1h, may make more than 4h
There is complicated reaction in leaching liquid, be unfavorable for obtaining extract；
S2：By the solution filtration that extracts and obtain, by the filtrate concentration being filtrated to get, medicinal extract is obtained；
S3：Products in water after the concentration is dissolved, the solution for the obtaining chromatographic column for being filled with AB-8 macroreticular resins
Adsorbing separation, the product are 1 with the mass ratio of the macroreticular resin:60～1:100, 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 for affording
The preferred scope determined with many factors such as recovery rates；Adsorption time is preferably 10h～14h, is that consideration adsorbing separation is
No abundant, so as to affect extract yield and extract activity；
S4：The chromatographic column is washed with water colourless to efflux, then with the volume fraction of 10～15 times of column volumes be
10%～80% ethanol water wash-out, collects ethanol eluate；
S5：By the ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
The preparation method of the white thorn antioxidative active extractive that the present invention is provided is made into one with reference to specific embodiment
Step explanation.
Embodiment one
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 30% by 15g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 4 hours, then the mixture of thorn dry fruit and ethanol water in vain is carried out ultrasonic extraction, ultrasound temperature
Spend for 40 DEG C, ultrasonic time is 60min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Embodiment two
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 50% by 15g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 4 hours, then the mixture of thorn dry fruit and ethanol water in vain is carried out ultrasonic extraction, ultrasound temperature
Spend for 40 DEG C, ultrasonic time is 60min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Embodiment three
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 70% by 15g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 4 hours, then the mixture of thorn dry fruit and ethanol water in vain is carried out ultrasonic extraction, ultrasound temperature
Spend for 40 DEG C, ultrasonic time is 60min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Example IV
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 95% by 15g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 4 hours, then the mixture of thorn dry fruit and ethanol water in vain is carried out ultrasonic extraction, ultrasound temperature
Spend for 40 DEG C, ultrasonic time is 60min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
The white thorn antioxidative active extractive that prepared according to above-described embodiment one to example IV carries out performance survey
Fixed, using anti-oxidant assay method (DPPH methods), concrete assay method is as follows：
(1) preparation of DPPH (1,1- diphenyl -2- trinitrophenyl-hydrazines) ethanol solution
Precision weighs 4mgDPPH powder, is placed in the volumetric flask of 50ml, adds absolute ethyl alcohol to scale, is configured to matter
Amount concentration is the solution of 80 μ g/ml, shakes up, 4 DEG C of refrigeration lucifuges, standby.
(2) preparation of testing sample and tester solution
Precision weighs appropriate testing sample and reference substance, with water or anhydrous alcohol solution and dilutes and is made into 5 variable concentrations
Solution (IC50 is within this concentration range), 4 DEG C refrigeration lucifuges, standby.Tester of the vitamin C for aqueous samples, dimension
Raw element E is the tester of fat-soluble sample.
(3) anti-oxidant assay method
By variable concentrations testing sample and reference substance solution, the DPPH ethanol solutions that 100 μ L add 80 μ g/mL are respectively taken
100 μ L, add a cover, shaking, avoid light place 30min mensuration absorbance value under 517nm.100 μ L samples solution and 100 μ LDPPH
The mixed liquor of ethanol solution, used as measure group；100 μ L samples solution and the mixed liquor of 100 μ L absolute ethyl alcohols, used as blank
Group；100 μ L samples solvents and the mixed liquor of 100 μ LDPPH solution, as a control group.
DPPH clearance rates (%)={ 1- (Asample-Ablamk)/Acontrol } × 100%
Asample：The absorbance (100 μ L) of the mixed liquor of sample solution (100 μ L)+DPPH solution
Ablank：The absorbance (100 μ L) of the mixed liquor of sample solution (100 μ L)+absolute ethyl alcohol
Acontrol：The absorbance (100 μ L) of the mixed liquor of sample solvent (100 μ L)+DPPH solution
With DPPH clearance rates (%) Y to sample solution mass concentration X, clearance rate curve is drawn, clearance rate and concentration is obtained
Linear equation, then calculate and try to achieve 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 antioxidation activity that the method that pressure homogeneous technology, membrane separation technique and macroreticular resin isolation technics combine is prepared is carried
Taking thing carries out performance measurement, and calculated extract yield and IC50 results are as shown in table 1 below：
The ethanol water result (n=3) of extract that obtain of the table 1 using different volumes fraction
| 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
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：Volume fraction by 5g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and 150mL is 70% second
Alcohol solution mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain is carried out homogenate extraction, homogenate extraction
Extraction time be 5 times, each extraction time of homogenate extraction is 1min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Embodiment six
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：Volume fraction by 5g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and 150mL is 70% second
Alcohol solution mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain is carried out ultrasonic extraction, ultrasonic temperature
For 40 DEG C, ultrasonic time is 60min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Embodiment seven
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：Volume fraction by 5g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and 150mL is 70% second
Alcohol solution mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain is carried out heating and refluxing extraction, heats
Return time is 1 hour；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Embodiment eight
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：Volume fraction by 5g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2014) and 150mL is 70% second
Alcohol solution mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain is carried out Microwave Extraction, Microwave Extraction
Time be 30min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then the volume fraction with 15 times of column volumes is 40% second
Alcohol solution is eluted, and collects ethanol eluate；
S5：By ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
Using above-mentioned same performance measurement method, the white thorn antioxygen prepared by above-described embodiment five to embodiment eight
Changing activity extract carries out performance measurement, and calculated extract yield and IC50 results are as shown in table 2 below：
Table 2 extracts the result (n=3) of the extract for obtaining using different extracting modes
| Embodiment | Extraction process | Extract yield | IC50(mg/mL) |
| Embodiment five | Sudden strain of a muscle is carried | 1.347% | 0.2630 |
| Embodiment six | Ultrasound | 1.579% | 0.2572 |
| Embodiment seven | Backflow | 1.032% | 0.3775 |
| Embodiment eight | Microwave | 0.968% | 0.4653 |
Embodiment nine
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 70% by 15g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2015) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain carried out homogenate extraction, flash carries
The extraction time for taking is 5 times, and homogenate extraction each extraction time is 1min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 10%,
20%th, 40%, 80% ethanol water wash-out, collects ethanol eluate respectively；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
Using above-mentioned same performance measurement method, above-described embodiment nine is eluted using the ethanol water of different volumes
The performance of the white thorn antioxidative active extractive for obtaining is measured, and calculated IC50 results are as shown in table 3 below：
The ethanol water wash-out result (n=3) of extract that obtain of the table 3 using different volumes fraction
| 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
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：By volume fraction of the 15g Nitraria sibirica dry fruits (is produced from the Inner Mongol, lot number NMG-2015) with 450mL it is
70% ethanol water mixing, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain is carried out homogenate extraction,
The extraction time of homogenate extraction is 5 times, and each extraction time of homogenate extraction is 1min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 10%,
20%th, 40%, 80% ethanol water wash-out, collects ethanol eluate respectively；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
Using above-mentioned same performance measurement method, above-described embodiment ten is eluted using the ethanol water of different volumes
The performance of the white thorn antioxidative active extractive for obtaining is measured, and calculated IC50 results are as shown in table 4 below：
The ethanol water wash-out result (n=3) of extract that obtain of the table 4 using different volumes fraction
| 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
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：Volume fraction by 385g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2015) and 11550mL is 70%
Ethanol water mixing, cold soaking 1 hour, then thorn dry fruit and the mixture of ethanol water in vain are carried out homogenate extraction is flash
The extraction time of extraction is 3 times, and each extraction time of homogenate extraction is 2min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, then respectively with the volume fraction of 15 times of column volumes be 10%,
40% ethanol water wash-out, collects ethanol eluate respectively；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
Using above-mentioned same performance measurement method, the ethanol aqueous wash for adopting different volumes to above-described embodiment 11
The performance of the de- white thorn antioxidative active extractive for obtaining is measured, and calculated IC50 results are as shown in table 5 below：
The ethanol water wash-out result (n=3) of extract that obtain of the table 5 using different volumes fraction
| Eluting liquid fraction | Extract yield | IC50(mg/mL) |
| 10% ethanol water | 7.267% | 0.248 |
| 40% ethanol water | 3.301% | 0.0485 |
Embodiment 12
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：Volume fraction by 385g Nitraria sibirica dry fruits (is produced from Qinghai, lot number QH2015) and 11550mL is 70%
Ethanol water mixing, cold soaking 1 hour, then thorn dry fruit and the mixture of ethanol water in vain are carried out homogenate extraction is flash
The extraction time of extraction is 3 times, and each extraction time of homogenate extraction is 2min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, be then 40% with the volume fraction of 15 times of column volumes respectively
Ethanol water wash-out, respectively collect ethanol eluate；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
The obtained antioxidation activity IC50 values for piercing antioxidative active extractive in vain are determined with DPPH methods as above is
0.049mg/mL, extractive content are 19.97g.
Embodiment 13
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 70% by 30g Nitraria sibirica dry fruits (is produced from Xinjiang, lot number XJ2015) and the volume fraction of 900mL
Ethanol water mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain carried out homogenate extraction, flash carries
The extraction time for taking is 3 times, and homogenate extraction each extraction time is 2min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, be then 40% with the volume fraction of 15 times of column volumes respectively
Ethanol water wash-out, respectively collect ethanol eluate；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
The obtained antioxidation activity IC50 values for piercing antioxidative active extractive in vain are determined with DPPH methods as above is
0.052mg/mL, extractive content are 0.86g.
Embodiment 14
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 70% by 30g Nitraria tangutorum dry fruits (is produced from the Inner Mongol, lot number NMG2015) and the volume fraction of 900mL
Ethanol water mixes, cold soaking 1 hour, then the mixture of thorn dry fruit and ethanol water in vain carried out homogenate extraction, flash carries
The extraction time for taking is 3 times, and each extraction time of homogenate extraction is 2min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:100, the time of adsorbing separation is 12h；
S4：Chromatographic column is washed with water colourless to efflux, be then 20% with the volume fraction of 15 times of column volumes respectively
Ethanol water wash-out, respectively collect ethanol eluate；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
The obtained antioxidation activity IC50 values for piercing antioxidative active extractive in vain are determined with DPPH methods as above is
0.10mg/mL, extractive content are 0.52g.
Embodiment 15
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 70% by 30g Nitraria tangutorum dry fruits (is produced from the Inner Mongol, lot number NMG2015) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 2 hours, then the mixture of thorn dry fruit and ethanol water in vain carried out homogenate extraction, flash carries
The extraction time for taking is 4 times, and each extraction time of homogenate extraction is 1.5min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:60, the time of adsorbing separation is 10h；
S4：Chromatographic column is washed with water colourless to efflux, be then 40% with the volume fraction of 10 times of column volumes respectively
Ethanol water wash-out, respectively collect ethanol eluate；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
The obtained antioxidation activity IC50 values for piercing antioxidative active extractive in vain are determined with DPPH methods as above is
0.097mg/mL, extractive content are 0.53g.
Embodiment 16
A kind of preparation method of white thorn antioxidative active extractive is present embodiments provided, is comprised the steps：
S1：It is 70% by 30g Nitraria tangutorum dry fruits (is produced from the Inner Mongol, lot number NMG2015) and the volume fraction of 450mL
Ethanol water mixes, cold soaking 2 hours, then the mixture of thorn dry fruit and ethanol water in vain carried out homogenate extraction, flash carries
The extraction time for taking is 4 times, and each extraction time of homogenate extraction is 1.5min；
S2：The solution filtration for obtaining will be extracted, the filtrate being filtrated to get is concentrated, medicinal extract is obtained；
S3：Products in water dissolving after by concentration, the solution for the obtaining chromatographic column absorption for being filled with AB-8 macroreticular resins
Separate, product is 1 with the mass ratio of macroreticular resin:80, the time of adsorbing separation is 14h；
S4：Chromatographic column is washed with water colourless to efflux, be then 40% with the volume fraction of 13 times of column volumes respectively
Ethanol water wash-out, respectively collect ethanol eluate；
S5：Ethanol eluate is distinguished concentrate drying, white thorn antioxidative active extractive is obtained.
The obtained antioxidation activity IC50 values for piercing antioxidative active extractive in vain are determined with DPPH methods as above is
0.078mg/mL, extractive content are 0.65g.
It should be noted that except situation about being enumerated to embodiment 16 from above-described embodiment one, other solid-liquid ratios, cold
Leaching time, wash-out ethanol water consumption, adsorption time, white thorn dry fruit species and the place of production are also feasible, are simply implementing
In the case that example one is enumerated to embodiment 16, the resultant effect of the activity of extract and extract yield is more preferable.
The preparation method of the white thorn antioxidative active extractive that the present invention is provided, can increase the yield of extract, improve
The antioxidation activity of white thorn antioxidative active extractive.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification, and does not make the essence of appropriate technical solution depart from various embodiments of the present invention skill
The scope of art scheme, its all should cover in the middle of the claim of the present invention and the scope of specification.
Claims (10)
1. a kind of preparation method of white thorn antioxidative active extractive, comprises the steps：
By thorn dry fruit in vain with the ethanol water that volume fraction is 30%～95% with 1g:The solid-liquid ratio mixing of (5～30) mL, cold
Leaching 1h～4h, then the mixture of the white thorn dry fruit and the ethanol water is extracted；
By the solution filtration that extracts and obtain, by the filtrate concentration being filtrated to get；
Products in water after the concentration is dissolved, the solution for the obtaining chromatographic column absorption point for being filled with AB-8 macroreticular resins
From the product is 1 with the mass ratio of the macroreticular resin:60～1:100；
The chromatographic column is washed with water colourless to efflux, then with the volume fraction of 10～15 times of column volumes be 10%～
80% ethanol water wash-out, collects ethanol eluate；
By the ethanol eluate concentrate drying, white thorn antioxidative active extractive is obtained.
2. according to claim 1 white thorn antioxidative active extractive preparation method, it is characterised in that：
The volume fraction of the ethanol water being used in mixed way is 50%～70%, and the solid-liquid ratio is 1g:30mL.
3. according to claim 1 white thorn antioxidative active extractive preparation method, it is characterised in that：
The extracting method of the extraction be heated to reflux, one or more in ultrasonic extraction, Microwave Extraction and homogenate extraction.
4. according to claim 3 white thorn antioxidative active extractive preparation method, it is characterised in that：
The extracting method is homogenate extraction, and the extraction time of the homogenate extraction is 3～5 times, the homogenate extraction each
Extraction time is 1min～2min.
5. according to claim 3 white thorn antioxidative active extractive preparation method, it is characterised in that：
The extracting method is ultrasonic extraction, and the ultrasonic temperature of the ultrasonic extraction is 40 DEG C, and ultrasonic time is 60min.
6. according to claim 1 white thorn antioxidative active extractive preparation method, it is characterised in that：
The time of the adsorbing separation is 10h～14h.
7. according to claim 1 white thorn antioxidative active extractive preparation method, it is characterised in that：
The volume fraction 20%～40% for eluting the ethanol water for using.
8. according to claim 1 white thorn antioxidative active extractive preparation method, it is characterised in that：
The white thorn dry fruit is Nitraria tangutorum dry fruit or Nitraria sibirica dry fruit.
9. the white thorn that the preparation method of the white thorn antioxidative active extractive according to any one of claim 1-8 is prepared
Antioxidative active extractive.
10. application of the white thorn antioxidative active extractive described in claim 9 in oxidation resistant product is prepared.
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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 |
| CN106975076A (en) * | 2017-04-14 | 2017-07-25 | 青岛市第三人民医院 | A kind of pepsin coating tablet containing Chinese medical extract |
| 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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