CN107641071A - A kind of method that mannitol is extracted from sea-tangle - Google Patents
A kind of method that mannitol is extracted from sea-tangle Download PDFInfo
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- CN107641071A CN107641071A CN201711152456.XA CN201711152456A CN107641071A CN 107641071 A CN107641071 A CN 107641071A CN 201711152456 A CN201711152456 A CN 201711152456A CN 107641071 A CN107641071 A CN 107641071A
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Abstract
The invention discloses a kind of method from sea-tangle extraction mannitol, it passes through following steps：（1）Fresh Laminaria Japonica is cut into silk；（2）It will be washed in the cleaning solution of Shredded kelp first that step 1 obtains, final filtration collects cleaning solution and Shredded kelp；（3）The Shredded kelp that step 2 obtains is washed in the second cleaning solution, final filtration collects cleaning solution and Shredded kelp；（4）The cleaning solution that combining step 2 and 3 obtains, and using NaOH solution regulation pH to 11 12, it is filtered to remove spawn；Then spawn is further filtered to remove using sulphur acid for adjusting pH to 67；（5）Be concentrated under reduced pressure extract solution, is filtered to remove insoluble component, cools down and adds ethanol, stirs and is cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain product.The method of the present invention can obtain the higher mannitol rate of recovery, and the extract solution used is less, reduces the harm to environment and wastewater treatment pressure.
Description
Technical field
The present invention relates to the extraction of hexahydroxylic alcohols, especially a kind of method that mannitol is extracted from sea-tangle.
Background technology
Sea-tangle（Scientific name：Laminaria japonica）, alias kelp, river Chinese cabbage, Phaeophyta Larminaria it is a kind of edible
Algae, eucaryon many cells.Sea-tangle originates in Northeast Asian region, including Russian pacific rim, Japan and NORTHERN KOREA edge
Sea, after grown in Chinese Liaodong Peninsula and the ocean of In Coastal Areas of Shandong, China, today, China was laminaria production state maximum in the world.Sea
Band spore is divided into holdfast, handle and strap three parts.
Mannitol is a kind of hexitol, pleasantly sweet because being absorbed heat during dissolving, has comfort sense to oral cavity, therefore be more widely used in awake
The manufacture of the chewable tablets such as freshener, its granular pattern are specially used as the excipient of direct tablet compressing in yeast for brewing rice wine, mouth.Mannitol is a kind of hypertonicity
Tissue dewatering agent, be clinically widely used in treating encephaledema, prevent acute renal failure, treat glaucoma, accelerate poisonous substance and medicine
Excretion of the thing from kidney.
Containing abundant mannitol composition in sea-tangle, mannitol is extracted from sea-tangle, be the modern Land use systems of sea-tangle it
One.
The content of the invention
In order to overcome deficiency of the prior art, it is an object of the invention to provide a kind of rate of recovery height, the extract solution used
Few method from sea-tangle extraction mannitol.
The technical solution adopted for the present invention to solve the technical problems is：A kind of method from sea-tangle extraction mannitol, its
It is characterised by：It passes through following steps：
（1）Fresh Laminaria Japonica is cut into the wide silks of 1-3mm；
（2）The Shredded kelp that step 1 obtains is washed into 90-120 in 60-80 degrees Celsius of 1.5-2 times of weight of the first cleaning solution
Minute, the first described cleaning solution includes 0.5-1.0% sodium carbonate, 0.5-1.0% ethanol by weight, and final filtration is collected and washed
Wash liquid and Shredded kelp；
（3）The Shredded kelp that step 2 obtains is washed into 90-120 in 20-40 degrees Celsius of 1.5-2 times of weight of the second cleaning solution
Minute, the second described cleaning solution includes 2.0-2.5% sodium carbonate, 0.5-1.0% ethanol by weight, and final filtration is collected and washed
Wash liquid and Shredded kelp；
（4）The cleaning solution that combining step 2 and 3 obtains, and using NaOH solution regulation pH to 11-12, it is filtered to remove gel
Material；Then spawn is further filtered to remove using sulphur acid for adjusting pH to 6-7；
（5）The extract solution that is concentrated under reduced pressure reaches the 20-25% of original volume, is filtered to remove insoluble component, is cooled to 60-70 degrees Celsius,
And the ethanol of 2-3 times of volume is added, stirs and is cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain production
Product.
In currently preferred aspect, in step 1, Fresh Laminaria Japonica is cut into the Shredded kelp of the wide wave-likes of 2mm.
In currently preferred aspect, in step 2, by the Shredded kelp that step 1 obtains at 75 degrees Celsius of 1.6 times of weight
The first cleaning solution in wash 100 minutes, the first described cleaning solution by weight including 0.75% sodium carbonate, 0.80% second
Alcohol, final filtration collect cleaning solution and Shredded kelp.
In currently preferred aspect, in step 3, by the Shredded kelp that step 2 obtains at 25 degrees Celsius of 1.6 times of weight
The second cleaning solution in wash 100 minutes, the second described cleaning solution by weight including 2.3% sodium carbonate, 0.80% ethanol,
Final filtration collects cleaning solution and Shredded kelp.
In currently preferred aspect, after step 3, the distillation water washing also including the use of 1.5-2 times of weight of use
Shredded kelp, and the cleaning solution that distillation water washing obtains is also incorporated into step 2 and 3 cleaning solution in step 4.
In currently preferred aspect, in step 2 and 3, it is ultrasonically treated in washing process.
In currently preferred aspect, in step 4, the cleaning solution that combining step 2 and 3 obtains, and use 30%
NaOH solution adjusts pH to 11.5, is filtered to remove spawn；Then using 10% sulphur acid for adjusting pH to 6.8, further mistake
Filter out spawn.
In currently preferred aspect, in steps of 5, the extract solution that is concentrated under reduced pressure reaches the 22% of original volume, is filtered to remove not
Soluble component, 66 degrees Celsius are cooled to, and add the ethanol of 2.5 times of volumes, stirred and be cooled to room temperature, centrifugation is received
Collect sediment, and be dried to obtain product.
In currently preferred aspect, after step 5, the step of also recrystallization including the use of ethanol.
The present invention from sea-tangle extraction mannitol method can obtain the higher rate of recovery, and the extract solution used compared with
It is few, reduce the harm to environment and wastewater treatment pressure.
Embodiment
Embodiment 1
In the present embodiment, prepared from the Fresh Laminaria Japonica of double centner, it is specifically, a kind of to extract mannitol from sea-tangle
Method, it passes through following steps：
（1）Fresh Laminaria Japonica is cut into the Shredded kelp of the wide wave-likes of 2mm；
（2）The Shredded kelp that step 1 obtains is washed 100 minutes in 75 degrees Celsius of the first cleaning solution of 1.6 times of weight, it is described
The first cleaning solution collect cleaning solution and Shredded kelp including 0.75% sodium carbonate, 0.80% ethanol, final filtration by weight；
（3）The Shredded kelp that step 2 obtains is washed 100 minutes in 25 degrees Celsius of the second cleaning solution of 1.6 times of weight, it is described
The second cleaning solution collect cleaning solution and Shredded kelp including 2.3% sodium carbonate, 0.80% ethanol, final filtration by weight；
（4）The cleaning solution that combining step 2 and 3 obtains, and using 30% NaOH solution regulation pH to 11.5, it is filtered to remove gel
Shape material；Then spawn is further filtered to remove using 10% sulphur acid for adjusting pH to 6.8；
（5）The extract solution that is concentrated under reduced pressure reaches the 22% of original volume, is filtered to remove insoluble component, is cooled to 66 degrees Celsius, and add
Enter the ethanol of 2.5 times of volumes, stir and be cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain product.
Embodiment 2
In the present embodiment, prepared from the Fresh Laminaria Japonica of double centner, a kind of method from sea-tangle extraction mannitol,
It passes through following steps：
（1）Fresh Laminaria Japonica is cut into the wide silks of 1mm；
（2）The Shredded kelp that step 1 obtains is washed 120 minutes in 60 degrees Celsius of the first cleaning solution of 2 times of weight, it is described
First cleaning solution collects cleaning solution and Shredded kelp including 1.0% sodium carbonate, 0.5% ethanol, final filtration by weight；
（3）The Shredded kelp that step 2 obtains is washed 120 minutes in 40 degrees Celsius of the second cleaning solution of 2 times of weight, it is described
Second cleaning solution collects cleaning solution and Shredded kelp including 2.5% sodium carbonate, 0.5% ethanol, final filtration by weight；
（4）The cleaning solution that combining step 2 and 3 obtains, and using NaOH solution regulation pH to 11, it is filtered to remove gelling material
Matter；Then spawn is further filtered to remove using sulphur acid for adjusting pH to 7；
（5）The extract solution that is concentrated under reduced pressure reaches the 20% of original volume, is filtered to remove insoluble component, is cooled to 60 degrees Celsius, and add
Enter the ethanol of 2 times of volumes, stir and be cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain product.
Embodiment 3
In the present embodiment, prepared from the Fresh Laminaria Japonica of double centner, a kind of method from sea-tangle extraction mannitol,
It passes through following steps：
（1）Fresh Laminaria Japonica is cut into the wide silks of 3mm；
（2）The Shredded kelp that step 1 obtains is washed 90 minutes in 80 degrees Celsius of the first cleaning solution of 1.5 times of weight, it is described
The first cleaning solution collect cleaning solution and Shredded kelp including 0.5% sodium carbonate, 1.0% ethanol, final filtration by weight；
（3）The Shredded kelp that step 2 obtains is washed 90 minutes in 20 degrees Celsius of the second cleaning solution of 1.5 times of weight, it is described
The second cleaning solution collect cleaning solution and Shredded kelp including 2.0% sodium carbonate, 1.0% ethanol, final filtration by weight；
（4）The cleaning solution that combining step 2 and 3 obtains, and using NaOH solution regulation pH to 12, it is filtered to remove gelling material
Matter；Then spawn is further filtered to remove using sulphur acid for adjusting pH to 6；
（5）The extract solution that is concentrated under reduced pressure reaches the 25% of original volume, is filtered to remove insoluble component, is cooled to 70 degrees Celsius, and add
Enter the ethanol of 3 times of volumes, stir and be cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain product.
Embodiment 4
In the present embodiment, being prepared from the Fresh Laminaria Japonica of double centner, its extracting method and embodiment 1 are substantially similar,
Difference is：
（1）After step 3, also including the use of the distillation water washing Shredded kelp using 1.7 times of weight, and in step 4 will
The cleaning solution that distillation water washing obtains is also incorporated into step 2 and 3 cleaning solution；
（2）In step 2 and 3, it is ultrasonically treated in washing process.
Embodiment 5
In the present embodiment, being prepared from the Fresh Laminaria Japonica of double centner, its extracting method and embodiment 1 are substantially similar,
Difference is：
（1）After step 3, also including the use of the distillation water washing Shredded kelp using 1.5 times of weight, and in step 4 will
The cleaning solution that distillation water washing obtains is also incorporated into step 2 and 3 cleaning solution；
（2）In step 2 and 3, it is ultrasonically treated in washing process.
Embodiment 6
In the present embodiment, being prepared from the Fresh Laminaria Japonica of double centner, its extracting method and embodiment 1 are substantially similar,
Difference is：
（1）After step 3, also including the use of the distillation water washing Shredded kelp using 2.0 times of weight, and in step 4 will
The cleaning solution that distillation water washing obtains is also incorporated into step 2 and 3 cleaning solution；
（2）In step 2 and 3, it is ultrasonically treated in washing process.
Comparative example 1
This comparative example is prepared from the Fresh Laminaria Japonica of double centner, and its extracting method and embodiment 1 are substantially similar, difference
It is：Step 3 is not performed, step 2 is performed twice, cleaning solution merges the processing for carrying out step 4.
Comparative example 2
This comparative example is prepared from the Fresh Laminaria Japonica of double centner, and its extracting method and embodiment 1 are substantially similar, difference
It is：Only sea-tangle is washed in step 2 and 3 using distilled water.
First, the yield of mannitol and the determination test of purity
In this experiment, the yield and purity of embodiment 1-6 and comparative example 1-2 mannitol are compared.The purity of mannitol is adopted
HPLC is taken to be measured（《The assay of mannitol in formula mannitol injection liquid（HPLC）》, China Health industry magazine, 2012
29 phases of year）, and be recorded in table 1.
Table 1：The yield and purity of embodiment 1-6 and comparative example 1-2 mannitol
| Group number | Yield/kilogram | Purity/wt.% |
| Embodiment 1 | 2.75 | 87.2% |
| Embodiment 2 | 2.66 | 85.1% |
| Embodiment 3 | 2.71 | 82.9% |
| Embodiment 4 | 3.21 | 87.4% |
| Embodiment 5 | 3.34 | 86.8% |
| Embodiment 6 | 2.97 | 87.1% |
| Comparative example 1 | 2.82 | 72.5% |
| Comparative example 2 | 2.46 | 81.7% |
From table 1 it can be appreciated that in embodiment 1-6 and in comparative example 1, higher yield can be obtained.But
The purity of comparative example 1 is significantly lower than other each groups.The mannitol yield and purity that embodiment 1-6, especially embodiment 4-6 are obtained
It is higher, realize preferable extraction effect.
2nd, the sea-tangle taste test after mannitol is extracted
In addition, the present inventor also surprisingly has found, embodiment 1-6 immersion after sea-tangle due to the medicament used be all can
As the medicament of food additives, its sea-tangle finally given has more crisp mouthfeel compared to comparative example 1-2, therefore will also implement
Example 1-6 method, especially embodiment 4-6 method are used as the preprocessing process of kelp food.In this preprocessing process,
Mannitol has not only been reclaimed, has also improved the food mouthfeel of sea-tangle.In order to verify this point, the present inventor recruited 10 it is tested
Person has carried out taste test to the sea-tangle of embodiment 1,4 and comparative example 1,2.Every subject is required to carry out four groups of sea-tangles
Taste and sort, and counted the more crisp mouthfeel of each group Shredded kelp（Most crisp is 4 points, secondly 3 points, and secondly 2 points, next 1
Point）.The scoring method can prevent the preference of some individual subjects and cause fraction too high or too low.As a result it is recorded in table
In 2.
Table 2：The taste test result of the sea-tangle of embodiment 1,4 and comparative example 1,2
| Group number | Taste score |
| Embodiment 1 | 35 |
| Embodiment 4 | 32 |
| Comparative example 1 | 20 |
| Comparative example 2 | 13 |
It can be seen that, the mouthfeel of embodiment 1,4 is than having clear and definite advantage for comparative example 1-2 from table 2.In view of comparative example
1 actually performs step 22 times, and mouthfeel should not be so poor in theory.This shows the washing step counterpart of low-temperature high-alkali
The lifting of sense is most important.
Claims (9)
- A kind of 1. method from sea-tangle extraction mannitol, it is characterised in that：It passes through following steps：（1）Fresh Laminaria Japonica is cut into the wide silks of 1-3mm；（2）The Shredded kelp that step 1 obtains is washed into 90-120 in 60-80 degrees Celsius of 1.5-2 times of weight of the first cleaning solution Minute, the first described cleaning solution includes 0.5-1.0% sodium carbonate, 0.5-1.0% ethanol by weight, and final filtration is collected and washed Wash liquid and Shredded kelp；（3）The Shredded kelp that step 2 obtains is washed into 90-120 in 20-40 degrees Celsius of 1.5-2 times of weight of the second cleaning solution Minute, the second described cleaning solution includes 2.0-2.5% sodium carbonate, 0.5-1.0% ethanol by weight, and final filtration is collected and washed Wash liquid and Shredded kelp；（4）The cleaning solution that combining step 2 and 3 obtains, and using NaOH solution regulation pH to 11-12, it is filtered to remove gel Material；Then spawn is further filtered to remove using sulphur acid for adjusting pH to 6-7；（5）The extract solution that is concentrated under reduced pressure reaches the 20-25% of original volume, is filtered to remove insoluble component, is cooled to 60-70 degrees Celsius, And the ethanol of 2-3 times of volume is added, stirs and is cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain production Product.
- A kind of 2. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：In step 1, will be new Fresh sea-tangle cuts into the Shredded kelp of the wide wave-likes of 2mm.
- A kind of 3. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：In step 2, will walk Rapid 1 obtained Shredded kelp washs 100 minutes in 75 degrees Celsius of 1.6 times of weight of the first cleaning solution, the described first washing Liquid collects cleaning solution and Shredded kelp including 0.75% sodium carbonate, 0.80% ethanol, final filtration by weight.
- A kind of 4. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：In step 3, will walk Rapid 2 obtained Shredded kelps wash 100 minutes in 25 degrees Celsius of 1.6 times of weight of the second cleaning solution, the described second washing Liquid collects cleaning solution and Shredded kelp including 2.3% sodium carbonate, 0.80% ethanol, final filtration by weight.
- A kind of 5. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：After step 3, also Including the use of the distillation water washing Shredded kelp using 1.5-2 times of weight, and the washing in step 4 obtaining distillation water washing Liquid is also incorporated into step 2 and 3 cleaning solution.
- A kind of 6. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：In step 2 and 3, It is ultrasonically treated in washing process.
- A kind of 7. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：In step 4, merge Step 2 and 3 obtained cleaning solutions, and using 30% NaOH solution regulation pH to 11.5, it is filtered to remove spawn；Then Using 10% sulphur acid for adjusting pH to 6.8, spawn is further filtered to remove.
- A kind of 8. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：In steps of 5, depressurize Concentrated extracting solution reaches the 22% of original volume, is filtered to remove insoluble component, is cooled to 66 degrees Celsius, and add 2.5 times of volumes Ethanol, stir and be cooled to room temperature, sediment is collected by centrifugation, and be dried to obtain product.
- A kind of 9. method from sea-tangle extraction mannitol according to claim 1, it is characterised in that：After step 5, also The step of being recrystallized including the use of ethanol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110663764A (en) * | 2019-11-20 | 2020-01-10 | 晋中学院 | Fruit and vegetable fresh-keeping coating containing moutan bark and preparation method thereof |
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| CN110663764A (en) * | 2019-11-20 | 2020-01-10 | 晋中学院 | Fruit and vegetable fresh-keeping coating containing moutan bark and preparation method thereof |
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Application publication date: 20180130 |