CN108840957A - A kind of extraction and purification process of garlic polysaccharide - Google Patents
A kind of extraction and purification process of garlic polysaccharide Download PDFInfo
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Abstract
The invention discloses a kind of extraction and purification processes of garlic polysaccharide, include the following steps：（1）Degreasing；（2）Ultrasonic treatment；（3）Enzymatic treatment；（4）Boiling；（5）Garlic polysaccharide extracting solution；（6）Alcohol precipitation；（7）Ion-exchange；（8）It is dry.The present invention uses specific complex enzyme, and it is aided with the method for ultrasound-assisted enzymolysis, it is significantly improved compared to common hot extraction recovery rate, garlic polysaccharide extracting solution is carried out ion exchange step by step by the present invention simultaneously, the purity of garlic polysaccharide is can effectively improve, to guarantee the present invention with higher extracted rate simultaneously, and can DNA purity with higher.
Description
Technical field
The present invention relates to garlics to process processing technique field, and in particular to a kind of extraction and purification process of garlic polysaccharide.
Background technique
Garlic is called garlic, garlic, giant garlic, calabash, only garlic, single clove garlic, is the general designation of garlic class plant.Semi-annual draft is planted
Object, Liliaceae allium, is used as medicine with bulb.Spring, summer harvesting, binding hang ventilation, dry in the shade spare.Farmer's proverb says " kind garlic not coldest days of the year end
（Month）, the coldest days of the year end long only head ", June leaf it is withered when excavate, remove silt, it is dry that crust is dried or is baked in ventilation.
Garlic is in oblate spheroid or short cone, and there are canescence or light brown film quality firecoat in outside, peel off scale leaf, inside there is 6-10
A garlic clove, wheel are born in around scape, and basal part of stem plate-like has most fibrous roots.Each garlic clove outsourcing film, peels off film, i.e.,
See the scale of white, plump succulence.There is the peppery gas of strong garlic, acrid flavour is peppery.Irritant smell, it is edible or for seasoning, also may be used
It is used as medicine.Underground bulb divides valve, is divided into purple skin kind and white skin kind by color of the leather difference.Garlic is Qin Hanshi from the incoming China in the Western Regions, is passed through
Artificial cultivation breeding has anticancer function, deep to be fond of by masses.
Garlic polysaccharide is the highest healthcare function ingredient of content in garlic, accounts for the 15%-25% of fresh garlic, has proliferation enteron aisle
Probiotics assists digestion, strengthen immunity, prevents hepatic injury, anti-oxidant and antiviral etc. multiple efficacies.Garlic polysaccharide is being cured
The fields such as medicine, food have wide actual application prospect.Currently, garlic polysaccharide volume extracting method is relatively simple, extract
Come garlic polysaccharide purity can not guarantee, meanwhile, the extracted amount of garlic polysaccharide is also far from the requirment.
In Chinese patent（Application number：CN98113263.4）A kind of extracting method of garlic polysaccharide is disclosed, including following
Step：A. it takes the peeling of garlic a batch to clean up, and is pounded mashed garlic；B. add 4 times of mashed garlic quality into mashed garlic
Water carry out boiling, with steam deodorization to release steam substantially without big garlic smell；C. by mashed garlic under the conditions of 95-100 DEG C
It boils and keeps the temperature 1 hour after half an hour, release cooking water；D. gained cooking water uses ammonium hydroxide through high speed centrifugation, film ultrafiltration concentration
It is adjusted to PH8,10%CaCl2 solution is added, is stirred 12 hours, high speed centrifugation obtains clear liquid again；E. gained clear liquid, it is dry greatly
Garlic polysaccharide (APS) white powder.Although operation is simple for the invention, and product purity is higher.But it is used in extraction process
The CaCl that fructose and levulan can be caused to precipitate2, this is unfavorable for the yield for improving garlic polysaccharide, while garlic polysaccharide purity
It is lower.
And in Chinese patent（Application number：CN201611000976.4）Disclose a kind of extraction purification side of garlic polysaccharide
Method, extracting method of the present invention is simple, easy to operate, high-efficient, price is low, optimizes the extraction work for preparing high-purity garlic polysaccharide
Skill isolates and purifies garlic polysaccharide fine work for scale and provides technical support, has good application value.But the invention makes
The extracted amount for the garlic polysaccharide that Hot water extraction extracts is relatively low.
Based on this, it is necessary to a kind of extraction and purification process of garlic polysaccharide is provided, to solve existing in the prior art ask
Topic.
Summary of the invention
In view of the above-mentioned analysis to the prior art, the present invention provides a kind of extraction and purification process of garlic polysaccharide, has and mentions
The advantage that rate is high, with high purity is taken, and extracting method is simple, it is easy to operate, high-efficient, it has good promotion and application value.
In order to achieve the above object, the present invention is achieved through the following technical solutions：
A kind of extraction and purification process of garlic polysaccharide, includes the following steps：
（1）Degreasing：Dry garlic is crushed, solvent degreasing is added in sieving, it flows back 2-5 times, 1-3 hours each, recycling design,
Residue air-dries；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 30-50 times of weight, super with 300-400W power
Sonication 15-35 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 50-70min at a temperature of 55-65 DEG C, then heats to 90 DEG C of enzyme deactivations,
It filters, collects filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
Preferably, the step（1）In, dry garlic is smashed it through into 50 meshes.
Preferably, the step（1）In, solvent is petroleum ether, and dosage is 10 times of weight of solid after sieving.
Preferably, the step（2）In, filter residue is soaked in the distilled water of 40 times of volumes and is ultrasonically treated, ultrasonic power
For 350W, ultrasonic time 20min.
Preferably, the step（3）In, addition complex enzyme be neutral proteinase, trypsase and flavor protease,
Weight is respectively 1.5%-2.0%, 1.5%-2.0% and 1.5%-2.0% of filter residue weight.
Preferably, the step（5）In, the liquid-to-solid ratio of the boiling mixed liquor of Hot water extraction heating is 8:1ml/g adds
Hot temperature is maintained at 95 DEG C, and extraction time is 2 hours.
Preferably, the step（5）In, to supernatant using be concentrated in vacuo, and by supernatant be concentrated into concentration before
1/10。
Preferably, the step（6）In, using the ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes to garlic polysaccharide
Extracting solution carries out alcohol precipitation processing and obtains crude polysaccharide powder, and the sedimentation time is 5 hours.
Preferably, the step（7）In, resin is using, simultaneously suction to allicin small to the adsorbance of garlic polysaccharide
Attached amount is big and is in the D315 macroreticular resin of reticular structure.
Preferably, the step（7）In, the elution speed to garlic crude polysaccharide powder is 2.0ml/min flow velocity.
Compared with prior art, the present invention having following beneficial effect：
（1）The present invention uses specific complex enzyme, and is aided with the method for ultrasound-assisted enzymolysis, extracts compared to common hot extraction
Rate significantly improves, while garlic polysaccharide extracting solution is carried out ion exchange step by step by the present invention, and it is more to have can effectively improve garlic
The purity of sugar, thus guarantee the present invention with higher extracted rate simultaneously, and can DNA purity with higher.
（2）The present invention improves the stability and dissolution rate of garlic polysaccharide by being concentrated under vacuum conditions.
（3）The extracting method of garlic polysaccharide of the invention is easy to operate, high-efficient, optimizes and prepares high-purity garlic polysaccharide
Extraction process, isolate and purify garlic polysaccharide fine work for scale and technical support be provided, have good application value.
Specific embodiment
Form by the following examples is described in further detail above content of the invention again, but should not be by this
The range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiment, all technologies based on realization belonging to above content of the present invention
It all belongs to the scope of the present invention.
Embodiment 1
The extraction and purification process of the garlic polysaccharide of the present embodiment, includes the following steps：
（1）Degreasing：Dry garlic is crushed, sieving, is added molten time, 1 hour every time, recycling design, residue air-dried；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 30 times of weight, with 300W power ultrasonic treatment
15 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 50min at a temperature of 55 DEG C, then heats to 90 DEG C of enzyme deactivations, filters, receives
Collect filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
Wherein, the step（1）In, dry garlic is smashed it through into 50 meshes.
Wherein, the step（1）In, solvent is petroleum ether, and dosage is 10 times of weight of solid after sieving.
Wherein, the step（3）In, addition complex enzyme is neutral proteinase, trypsase and flavor protease, weight
Respectively 1.5%, 1.5% and the 1.5%% of filter residue weight.
Wherein, the step（5）In, the liquid-to-solid ratio of the boiling mixed liquor of Hot water extraction heating is 8:1ml/g, heating temperature
Degree is maintained at 95 DEG C, and extraction time is 2 hours.
Wherein, the step（5）In, to supernatant using vacuum concentration, and supernatant is concentrated into 1/10 before being concentrated.
Wherein, the step（6）In, garlic polysaccharide is extracted using the ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes
Liquid carries out alcohol precipitation processing and obtains crude polysaccharide powder, and the sedimentation time is 5 hours.
Wherein, the step（7）In, resin is using adsorbance small to the adsorbance of garlic polysaccharide while to allicin
D315 macroreticular resin that is big and being in reticular structure.
Wherein, the step（7）In, the elution speed to garlic crude polysaccharide powder is 2.0ml/min flow velocity.
Embodiment 2
The extraction and purification process of the garlic polysaccharide of the present embodiment, includes the following steps：
（1）Degreasing：Dry garlic is crushed, solvent degreasing is added in sieving, it flows back 5 times, 3 hours every time, recycling design, residue
It air-dries；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 50 times of weight, with 400W power ultrasonic treatment
35 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 70min at a temperature of 65 DEG C, then heats to 90 DEG C of enzyme deactivations, filters, receives
Collect filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
Wherein, the step（1）In, dry garlic is smashed it through into 50 meshes.
Wherein, the step（1）In, solvent is petroleum ether, and dosage is 10 times of weight of solid after sieving.
Wherein, the step（3）In, addition complex enzyme is neutral proteinase, trypsase and flavor protease, weight
Respectively 2.0%, 2.0% and the 2.0% of filter residue weight.
Wherein, the step（5）In, the liquid-to-solid ratio of the boiling mixed liquor of Hot water extraction heating is 8:1ml/g, heating temperature
Degree is maintained at 95 DEG C, and extraction time is 2 hours.
Wherein, the step（5）In, to supernatant using vacuum concentration, and supernatant is concentrated into 1/10 before being concentrated.
Wherein, the step（6）In, garlic polysaccharide is extracted using the ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes
Liquid carries out alcohol precipitation processing and obtains crude polysaccharide powder, and the sedimentation time is 5 hours.
Wherein, the step（7）In, resin is using adsorbance small to the adsorbance of garlic polysaccharide while to allicin
D315 macroreticular resin that is big and being in reticular structure.
Wherein, the step（7）In, the elution speed to garlic crude polysaccharide powder is 2.0ml/min flow velocity.
Embodiment 3
The extraction and purification process of the garlic polysaccharide of the present embodiment, includes the following steps：
（1）Degreasing：Dry garlic is crushed, solvent degreasing is added in sieving, it flows back 3 times, 2 hours every time, recycling design, residue
It air-dries；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 40 times of weight, with 350W power ultrasonic treatment
20 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 60min at a temperature of 60 DEG C, then heats to 90 DEG C of enzyme deactivations, filters, receives
Collect filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
Wherein, the step（1）In, dry garlic is smashed it through into 50 meshes.
Wherein, the step（1）In, solvent is petroleum ether, and dosage is 10 times of weight of solid after sieving.
Wherein, the step（3）In, addition complex enzyme is neutral proteinase, trypsase and flavor protease, weight
Respectively 1.5%-2.0%, 1.5%-2.0% and 1.5%-2.0% of filter residue weight.
Wherein, the step（5）In, the liquid-to-solid ratio of the boiling mixed liquor of Hot water extraction heating is 8:1ml/g, heating temperature
Degree is maintained at 95 DEG C, and extraction time is 2 hours.
Wherein, the step（5）In, to supernatant using vacuum concentration, and supernatant is concentrated into 1/10 before being concentrated.
Wherein, the step（6）In, garlic polysaccharide is extracted using the ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes
Liquid carries out alcohol precipitation processing and obtains crude polysaccharide powder, and the sedimentation time is 5 hours.
Wherein, the step（7）In, resin is using adsorbance small to the adsorbance of garlic polysaccharide while to allicin
D315 macroreticular resin that is big and being in reticular structure.
Wherein, the step（7）In, the elution speed to garlic crude polysaccharide powder is 2.0ml/min flow velocity.
Embodiment 4
The extraction and purification process of the garlic polysaccharide of the present embodiment, includes the following steps：
（1）Degreasing：Dry garlic is crushed, solvent degreasing is added in sieving, flows back 4 times, 2.5 hours every time, recycling design was residual
Slag air-dries；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 45 times of weight, with 380W power ultrasonic treatment
30 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 65min at a temperature of 63 DEG C, then heats to 90 DEG C of enzyme deactivations, filters, receives
Collect filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
Wherein, the step（1）In, dry garlic is smashed it through into 50 meshes.
Wherein, the step（1）In, solvent is petroleum ether, and dosage is 10 times of weight of solid after sieving.
Wherein, the step（3）In, addition complex enzyme is neutral proteinase, trypsase and flavor protease, weight
Respectively 1.8%, 1.8% and the 1.9% of filter residue weight.
Wherein, the step（5）In, the liquid-to-solid ratio of the boiling mixed liquor of Hot water extraction heating is 8:1ml/g, heating temperature
Degree is maintained at 95 DEG C, and extraction time is 2 hours.
Wherein, the step（5）In, to supernatant using vacuum concentration, and supernatant is concentrated into 1/10 before being concentrated.
Wherein, the step（6）In, garlic polysaccharide is extracted using the ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes
Liquid carries out alcohol precipitation processing and obtains crude polysaccharide powder, and the sedimentation time is 5 hours.
Wherein, the step（7）In, resin is using adsorbance small to the adsorbance of garlic polysaccharide while to allicin
D315 macroreticular resin that is big and being in reticular structure.
Wherein, the step（7）In, the elution speed to garlic crude polysaccharide powder is 2.0ml/min flow velocity.
Embodiment 5
The extraction and purification process of the garlic polysaccharide of the present embodiment, includes the following steps：
（1）Degreasing：Dry garlic is crushed, solvent degreasing is added in sieving, flows back 3 times, 1.5 hours every time, recycling design was residual
Slag air-dries；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 35 times of weight, with 320W power ultrasonic treatment
20 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 55min at a temperature of 58 DEG C, then heats to 90 DEG C of enzyme deactivations, filters, receives
Collect filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
Wherein, the step（1）In, dry garlic is smashed it through into 50 meshes.
Wherein, the step（1）In, solvent is petroleum ether, and dosage is 10 times of weight of solid after sieving.
Wherein, the step（3）In, addition complex enzyme is neutral proteinase, trypsase and flavor protease, weight
Respectively 1.6%, 1.9% and the 1.6% of filter residue weight.
Wherein, the step（5）In, the liquid-to-solid ratio of the boiling mixed liquor of Hot water extraction heating is 8:1ml/g, heating temperature
Degree is maintained at 95 DEG C, and extraction time is 2 hours.
Wherein, the step（5）In, to supernatant using vacuum concentration, and supernatant is concentrated into 1/10 before being concentrated.
Wherein, the step（6）In, garlic polysaccharide is extracted using the ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes
Liquid carries out alcohol precipitation processing and obtains crude polysaccharide powder, and the sedimentation time is 5 hours.
Wherein, the step（7）In, resin is using adsorbance small to the adsorbance of garlic polysaccharide while to allicin
D315 macroreticular resin that is big and being in reticular structure.
Wherein, the step（7）In, the elution speed to garlic crude polysaccharide powder is 2.0ml/min flow velocity.
Comparative example 1
Using Chinese patent（Application number：CN98113263.4）In method made from garlic polysaccharide.
Comparative example 2
Using Chinese patent（Application number：CN201611000976.4）In method made from garlic polysaccharide.
Comparative example 3
Ultrasonic treatment is not used：Save ultrasonic treatment, handled by the way of conventional stirring, other steps and method with
Embodiment 3 is consistent.
Comparative example 4
Ion-exchange is not used to handle：Ion-exchange processing is saved, is handled using conventional filtering suction type, other steps and method
It is consistent with embodiment 3.
Comparative example 5
Use neutral proteinase, other steps and method and embodiment 3 consistent merely.
Comparative example 6
Use trypsase, other steps and method and embodiment 3 consistent merely.
Comparative example 7
Use flavor protease, other steps and method and embodiment 3 consistent merely.
Experimental example 1
The purity of the garlic polysaccharide recovery rate of embodiment 1-5 and comparative example 1-4, the garlic polysaccharide of extraction is detected, as a result
Shown in table 1：
Table 1
| Project | Recovery rate（%） | Purity（%） |
| Embodiment 1 | 65 | 97.8 |
| Embodiment 2 | 67 | 98.5 |
| Embodiment 3 | 69 | 96.5 |
| Embodiment 4 | 72 | 97.3 |
| Embodiment 5 | 66 | 98.9 |
| Comparative example 1 | 38 | 84.5 |
| Comparative example 2 | 49 | 87.5 |
| Comparative example 3 | 54 | 95.4 |
| Comparative example 4 | 62 | 89.8 |
As shown in Table 1：
1, the recovery rate of garlic polysaccharide of the invention and purity are better than the prior art.
If 2, not using ultrasonic treatment, it can be seen that the quality of the garlic polysaccharide of extraction is greatly reduced.
If 3, not using ion-exchange to handle, it can be seen that the purity of the garlic polysaccharide of extraction is greatly reduced.
Experimental example 2
The purity of the garlic polysaccharide recovery rate of embodiment 3 and comparative example 5-7, the garlic polysaccharide of extraction is detected, as a result table 2
It is shown：
Table 2
| Project | Recovery rate（%） |
| Embodiment 5 | 70 |
| Comparative example 5 | 45 |
| Comparative example 6 | 49 |
| Comparative example 7 | 47 |
As shown in Table 2, under equal conditions, using complex enzyme（Neutral proteinase, trypsase, flavor protease）The material of processing
Compared with the material using single enzymatic treatment, the garlic polysaccharide of extraction is more.
In conclusion the present invention uses specific complex enzyme, and it is aided with the method for ultrasound-assisted enzymolysis, compares ordinary hot
Extraction method recovery rate significantly improves, while garlic polysaccharide extracting solution is carried out ion exchange step by step by the present invention, can effectively be mentioned
The high purity of garlic polysaccharide, thus guarantee the present invention with higher extracted rate simultaneously, and can DNA purity with higher.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of extraction and purification process of garlic polysaccharide, which is characterized in that include the following steps：
（1）Degreasing：Dry garlic is crushed, solvent degreasing is added in sieving, it flows back 2-5 times, 1-3 hours each, recycling design,
Residue air-dries；
（2）Ultrasonic treatment：By step（1）Gained filter residue is soaked in the distilled water of 30-50 times of weight, super with 300-400W power
Sonication 15-35 minutes, obtain solid-liquid mixture；
（3）Enzymatic treatment：Complex enzyme is added, then hydrolyzes 50-70min at a temperature of 55-65 DEG C, then heats to 90 DEG C of enzyme deactivations,
It filters, collects filtrate, concentration obtains concentrated extracting solution；
（4）Boiling：It is heated using Boiler Steam, and steam is directly passed through in concentrated extracting solution, distilled into concentrated extracting solution
Until there is no garlic smell, boiling mixed liquor is obtained；
（5）Garlic polysaccharide extracting solution：Boiling mixed liquor is centrifuged, residue is used into hot water extraction again after obtaining residue and is centrifuged,
Merge supernatant twice, supernatant is concentrated, obtains garlic polysaccharide extracting solution；
（6）Alcohol precipitation：Garlic polysaccharide extracting solution is subjected to alcohol precipitation processing, garlic Thick many candies therein are separated, it is on the one hand de-
Except partial impurities, while obtaining garlic crude polysaccharide powder；
（7）Ion-exchange：Garlic crude polysaccharide powder is isolated and purified into removal free allicin therein using ion-exchange chromatography, is removed
A small amount of pigment and small molecular weight impurity are removed using decoloration and dialysis, finally obtain garlic polysaccharide by the polysaccharide after allicin；
（8）It is dry：Garlic polysaccharide is spray-dried, the garlic polysaccharide product of white powder is obtained.
2. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（1）In, it will do
Dry garlic smashes it through 50 meshes.
3. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（1）In, solvent
For petroleum ether, and dosage is 10 times of weight of solid after sieving.
4. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（2）In, filter residue
It is soaked in the distilled water of 40 times of volumes and is ultrasonically treated, ultrasonic power 350W, ultrasonic time 20min.
5. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（3）In, it is added
Complex enzyme is neutral proteinase, trypsase and flavor protease, and weight is respectively 1.5%-2.0%, 1.5%- of filter residue weight
2.0% and 1.5%-2.0%.
6. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（5）In, hot water
The liquid-to-solid ratio of the boiling mixed liquor of extraction heating is 8:1ml/g, heating temperature are maintained at 95 DEG C, and extraction time is 2 hours.
7. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（5）In, to upper
Clear liquid is concentrated into 1/10 before being concentrated using vacuum concentration, and by supernatant.
8. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（6）In, it uses
The ethanol solution of 3 times of garlic polysaccharide extracting liquid volumes carries out alcohol precipitation processing to garlic polysaccharide extracting solution and obtains crude polysaccharide powder, precipitating
Time is 5 hours.
9. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（7）In, resin
While large amount of adsorption to allicin small using the adsorbance to garlic polysaccharide and the D315 macroreticular resin in reticular structure.
10. the extraction and purification process of garlic polysaccharide according to claim 1, which is characterized in that the step（7）In, it is right
The elution speed of garlic crude polysaccharide powder is 2.0ml/min flow velocity.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518660A (en) * | 2020-04-29 | 2020-08-11 | 劲牌有限公司 | Health-care white spirit with effect of relieving alcoholic brain injury and preparation method thereof |
| CN112375155A (en) * | 2020-11-11 | 2021-02-19 | 佛山科学技术学院 | Young garlic shoot polysaccharide and preparation method and application thereof |
| CN112812196A (en) * | 2019-11-18 | 2021-05-18 | 晨光生物科技集团股份有限公司 | Industrial method for producing garlic polysaccharide by using garlic processing waste |
| CN114558027A (en) * | 2022-03-15 | 2022-05-31 | 山东农业大学 | Preparation method and application of garlic polysaccharide-zinc compound |
-
2018
- 2018-05-31 CN CN201810546941.3A patent/CN108840957A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112812196A (en) * | 2019-11-18 | 2021-05-18 | 晨光生物科技集团股份有限公司 | Industrial method for producing garlic polysaccharide by using garlic processing waste |
| CN111518660A (en) * | 2020-04-29 | 2020-08-11 | 劲牌有限公司 | Health-care white spirit with effect of relieving alcoholic brain injury and preparation method thereof |
| CN112375155A (en) * | 2020-11-11 | 2021-02-19 | 佛山科学技术学院 | Young garlic shoot polysaccharide and preparation method and application thereof |
| CN114558027A (en) * | 2022-03-15 | 2022-05-31 | 山东农业大学 | Preparation method and application of garlic polysaccharide-zinc compound |
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