CN101704720B - Preparation method of mannitol - Google Patents
Preparation method of mannitol Download PDFInfo
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- CN101704720B CN101704720B CN2009102329915A CN200910232991A CN101704720B CN 101704720 B CN101704720 B CN 101704720B CN 2009102329915 A CN2009102329915 A CN 2009102329915A CN 200910232991 A CN200910232991 A CN 200910232991A CN 101704720 B CN101704720 B CN 101704720B
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- preparation
- usp mannitol
- ethanol
- filtering
- concentrates
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 title claims abstract description 27
- 229930195725 Mannitol Natural products 0.000 title claims abstract description 26
- 235000010355 mannitol Nutrition 0.000 title claims abstract description 26
- 239000000594 mannitol Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 241000830535 Ligustrum lucidum Species 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims description 21
- 230000006837 decompression Effects 0.000 claims description 14
- 238000004064 recycling Methods 0.000 claims description 14
- 230000000274 adsorptive effect Effects 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 7
- 238000001640 fractional crystallisation Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 235000014347 soups Nutrition 0.000 claims description 7
- 239000003463 adsorbent Substances 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 6
- 239000000706 filtrate Substances 0.000 abstract 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 230000003321 amplification Effects 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- 239000003480 eluent Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000003199 nucleic acid amplification method Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 241000201295 Euphrasia Species 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002934 diuretic Substances 0.000 description 1
- 230000001882 diuretic effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of mannitol, which has simple and convenient operation, and less pollution and device investment. The method comprises the following processing steps: taking and crushing glossy privet leaves, adding 70-95% ethanol with of the volume of the 5-10 times of weight of the glossy privet leaves, heating and conducting reflux for 2-4 times with 1-3 hours each time, merging liquid medicine, filtering, recovering and concentrating the ethanol by reducing pressure, refrigerating for 8-20 hours, filtering, collecting filtrate, adsorbing by using a large pore resin column, eluting by using 30-90% ethanol, collecting eluent with the amount of 3-8 times of the volume of the column, adjusting pH to be 10-11 by using stronger ammonia water, filtering, taking the filtrate, recovering and concentrating the ethanol by reducing pressure, standing overnight, filtering, taking filter residue, adding anhydrous ethanol and dissolving, decoloring by using activated carbon, filtering, concentrating the filtrate, and standing for crystallization. The mannitol prepared by the preparation method has high product purity, and is easy to realize industrialized amplification.
Description
Technical field
The present invention relates to a kind of preparation method of N.F,USP MANNITOL, especially a kind of method of from plant, extracting N.F,USP MANNITOL.
Background technology
N.F,USP MANNITOL (Mannitol), different name D-N.F,USP MANNITOL etc., molecular formula: C
6H
14O
6, molecular weight: 182.173, CAS accession number: 69-65-8, structural formula is following:
N.F,USP MANNITOL is a kind of natural compounds, can be used as sweeting agent, diuretic(s) etc., extensively is present in the various plants.
Leaf of Glossy Privet is the blade of Oleaceae plant glossy privet Ligustrum lucidum Ait., has and dispels the wind, make eye bright, and detumescence, effects such as pain relieving wherein contain a large amount of N.F,USP MANNITOL.
In the prior art, the extraction separation of N.F,USP MANNITOL mainly adopts organic solvent method etc., but the content of the N.F,USP MANNITOL that these extraction processes obtain is low, and is seriously polluted in the production process, and unfavorable big production operation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, N.F,USP MANNITOL that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get Leaf of Glossy Privet, pulverize, add 70-95% alcohol heating reflux 2-4 time that its weight 5-10 doubly measures volume, each 1-3 hour, merge soup, filtration; Decompression recycling ethanol also concentrates, and refrigerates 8-20 hour, filters, and collects filtrating, through macroporous adsorptive resins absorption, uses the 30-90% ethanol elution; Collect 3-8 times of column volume amount elutriant, strong aqua is regulated pH10-11, filters, and gets filtrating, and decompression recycling ethanol also concentrates; Placement is spent the night, and filters, and gets filter residue, adds anhydrous alcohol solution, activated carbon decolorizing; Filter, filtrating concentrates, and places crystallization, and fractional crystallization washs, is drying to obtain.
The alcohol heating reflux condition optimization is: add 85% alcohol heating reflux 3 times of 8 times of its weight amount volume, each 2 hours.
The time of refrigeration is preferably 12 hours.
The model of macroporous adsorbent resin is one or more among AB-8, H-103, D-101, DA-201, the DS-401.
The alcohol concn of wash-out macroporous adsorptive resins is preferably 60%.
The amount of collecting the macroporous adsorptive resins elutriant is 5 times of amount column volumes.
Adopt technique scheme to prepare N.F,USP MANNITOL, easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
To combine embodiment that the present invention is done further elaboration below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1
Get Leaf of Glossy Privet 10Kg, pulverize, add 70% alcohol heating reflux 2 times of 5 times of amounts of its weight volume, each 1 hour, merge soup, filter; Decompression recycling ethanol also concentrates, and refrigerates 8 hours, filters, and collects filtrating, through the absorption of AB-8 macroporous adsorptive resins, uses 30% ethanol elution; Collect 3 times of column volume amount elutriants, strong aqua is regulated pH10-11, filters, and gets filtrating, and decompression recycling ethanol also concentrates, and placement is spent the night; Filter, get filter residue, add anhydrous alcohol solution, activated carbon decolorizing filters, and filtrating concentrates; Place crystallization, fractional crystallization washs, is drying to obtain N.F,USP MANNITOL 42.1g, detects through HPLC, and purity is 98.3%.
Embodiment 2
Get Leaf of Glossy Privet 10Kg, pulverize, add 95% alcohol heating reflux 4 times of 10 times of amounts of its weight volume, each 3 hours, merge soup, filter; Decompression recycling ethanol also concentrates, and refrigerates 20 hours, filters, and collects filtrating, through the absorption of H-103 macroporous adsorptive resins, uses 90% ethanol elution; Collect 8 times of column volume amount elutriants, strong aqua is regulated pH10-11, filters, and gets filtrating, and decompression recycling ethanol also concentrates, and placement is spent the night; Filter, get filter residue, add anhydrous alcohol solution, activated carbon decolorizing filters, and filtrating concentrates; Place crystallization, fractional crystallization washs, is drying to obtain N.F,USP MANNITOL 61.8g, detects through HPLC, and purity is 98.6%.
Embodiment 3
Get Leaf of Glossy Privet 10Kg, pulverize, add 85% alcohol heating reflux 3 times of 8 times of amounts of its weight volume, each 2 hours, merge soup, filter; Decompression recycling ethanol also concentrates, and refrigerates 12 hours, filters, and collects filtrating, through the absorption of D101 macroporous adsorptive resins, uses 60% ethanol elution; Collect 5 times of column volume amount elutriants, strong aqua is regulated pH10-11, filters, and gets filtrating, and decompression recycling ethanol also concentrates, and placement is spent the night; Filter, get filter residue, add anhydrous alcohol solution, activated carbon decolorizing filters, and filtrating concentrates; Place crystallization, fractional crystallization washs, is drying to obtain N.F,USP MANNITOL 52.3g, detects through HPLC, and purity is 99.2%.
Embodiment 4
Get Leaf of Glossy Privet 10Kg, pulverize, add 85% alcohol heating reflux 3 times of 8 times of amounts of its weight volume, each 2 hours, merge soup, filter; Decompression recycling ethanol also concentrates, and refrigerates 12 hours, filters, and collects filtrating, through the absorption of DA-201 macroporous adsorptive resins, uses 60% ethanol elution; Collect 5 times of column volume amount elutriants, strong aqua is regulated pH10-11, filters, and gets filtrating, and decompression recycling ethanol also concentrates, and placement is spent the night; Filter, get filter residue, add anhydrous alcohol solution, activated carbon decolorizing filters, and filtrating concentrates; Place crystallization, fractional crystallization washs, is drying to obtain N.F,USP MANNITOL 51.1g, detects through HPLC, and purity is 99.0%.
Embodiment 5
Get Leaf of Glossy Privet 10Kg, pulverize, add 85% alcohol heating reflux 3 times of 8 times of amounts of its weight volume, each 2 hours, merge soup, filter; Decompression recycling ethanol also concentrates, and refrigerates 12 hours, filters, and collects filtrating, through the absorption of DS-401 macroporous adsorptive resins, uses 60% ethanol elution; Collect 5 times of column volume amount elutriants, strong aqua is regulated pH10-11, filters, and gets filtrating, and decompression recycling ethanol also concentrates, and placement is spent the night; Filter, get filter residue, add anhydrous alcohol solution, activated carbon decolorizing filters, and filtrating concentrates; Place crystallization, fractional crystallization washs, is drying to obtain N.F,USP MANNITOL 50.0g, detects through HPLC, and purity is 98.8%.
Claims (6)
1. the preparation method of a N.F,USP MANNITOL is characterized in that described method comprises the following steps: to get Leaf of Glossy Privet, pulverizes, and adds 70-95% alcohol heating reflux 2-4 time that its weight 5-10 doubly measures volume, 1-3 hour at every turn; Merge soup, filter, decompression recycling ethanol also concentrates, and refrigerates 8-20 hour, filters; Collect filtrating, through macroporous adsorptive resins absorption, use the 30-90% ethanol elution, collect 3-8 times of column volume amount elutriant, strong aqua is regulated pH10-11; Filter, get filtrating, decompression recycling ethanol also concentrates, and placement is spent the night, and filters; Get filter residue, add anhydrous alcohol solution, activated carbon decolorizing filters; Filtrating concentrates, and places crystallization, and fractional crystallization washs, is drying to obtain.
2. according to the preparation method of the said N.F,USP MANNITOL of claim 1, it is characterized in that described alcohol heating reflux condition is: add 85% alcohol heating reflux 3 times of 8 times of its weight amount volume, each 2 hours.
3. according to the preparation method of the said N.F,USP MANNITOL of claim 1, the time that it is characterized in that said refrigeration is 12 hours.
4. according to the preparation method of the said N.F,USP MANNITOL of claim 1, the model that it is characterized in that said macroporous adsorbent resin is one or more among AB-8, H-103, D-101, DA-201, the DS-401.
5. according to the preparation method of the said N.F,USP MANNITOL of claim 1, the alcohol concn that it is characterized in that said wash-out macroporous adsorptive resins is 60%.
6. according to the preparation method of the said N.F,USP MANNITOL of claim 1, the amount that it is characterized in that said collection macroporous adsorptive resins elutriant is 5 times of amount column volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102329915A CN101704720B (en) | 2009-10-20 | 2009-10-20 | Preparation method of mannitol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102329915A CN101704720B (en) | 2009-10-20 | 2009-10-20 | Preparation method of mannitol |
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| Publication Number | Publication Date |
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| CN101704720A CN101704720A (en) | 2010-05-12 |
| CN101704720B true CN101704720B (en) | 2012-11-21 |
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| CN2009102329915A Active CN101704720B (en) | 2009-10-20 | 2009-10-20 | Preparation method of mannitol |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297796B (en) * | 2010-06-23 | 2015-09-09 | 天津天士力之骄药业有限公司 | The fast separating process of sweet mellow wine and other water soluble ingredients in solid potpourri |
| CN105152861B (en) * | 2015-09-11 | 2017-06-06 | 中国科学院过程工程研究所 | A kind of method that mannitol is prepared in the oligosaccharide syrup from saline cistanche |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053580A (en) * | 2006-11-10 | 2007-10-17 | 燕山大学 | New medical application of traditional Chinese medicine privet and preparation method of its extraction |
-
2009
- 2009-10-20 CN CN2009102329915A patent/CN101704720B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053580A (en) * | 2006-11-10 | 2007-10-17 | 燕山大学 | New medical application of traditional Chinese medicine privet and preparation method of its extraction |
Non-Patent Citations (4)
| Title |
|---|
| 女贞子化学成分的研究;程晓芳等;《中国药科大学学报》;20001231;第31卷(第3期);第169-170页 * |
| 小叶女贞化学成分研究;李晓蒙等;《广东药学院学报》;19981231;第14卷(第2期);第93-94页 * |
| 李晓蒙等.小叶女贞化学成分研究.《广东药学院学报》.1998,第14卷(第2期),第93-94页. |
| 程晓芳等.女贞子化学成分的研究.《中国药科大学学报》.2000,第31卷(第3期),第169-170页. |
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| CN101704720A (en) | 2010-05-12 |
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