CN102399129A - Method for extracting 1-octacosanol from bagasse - Google Patents
Method for extracting 1-octacosanol from bagasse Download PDFInfo
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- CN102399129A CN102399129A CN2011103628818A CN201110362881A CN102399129A CN 102399129 A CN102399129 A CN 102399129A CN 2011103628818 A CN2011103628818 A CN 2011103628818A CN 201110362881 A CN201110362881 A CN 201110362881A CN 102399129 A CN102399129 A CN 102399129A
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Abstract
The invention discloses a method for extracting 1-octacosanol from bagasse. The method is characterized by comprising the following steps of: (1) grinding the bagasse into powder; (2) putting the bagasse powder obtained in the step (1) into an extraction kettle to form a packing layer; (3) extracting, namely introducing supercritical carbon dioxide into the extraction kettle through the bottom of the extraction kettle, allowing the supercritical carbon dioxide to flow through the bagasse powder of the packing layer, flow out of the extraction kettle through the top of the extraction kettle and enter a separation kettle, and performing ultrasonic radiation on the supercritical carbon dioxide in the extraction kettle in the extracting process; and (4) separating 1-octacosanol dissolved in the carbon dioxide in the separation kettle. The 1-octacosanol is extracted by an ultrasound-enhanced supercritical carbon dioxide fluid, so the production efficiency is high, the cost is low, the product purity is high, organic solvents are not contained, and the 1-octacosanol can serve as an important raw material for health foods, cosmetics and medicines.
Description
Technical field
The present invention relates to the deep process technology field of natural product, be specifically related to the method for policosanol in a kind of ultrasound-enhanced supercritical carbon dioxide abstraction bagasse.
Background technology
Policosanol is naturally occurring higher alcohols, mainly is present in cerosin, chaff wax, and wheatgerm oil is in the natural products such as beeswax and insect wax.Policosanol is a kind of safe, nutritional type supplement efficiently, has many biological functions and clinical value, can be used for treating the osteoporosis of hypercalcemia, treatment hypercholesterolemia and teinemia disease, the sexual behaviour that stimulates the animal and the mankind.The makeup that contain policosanol can promote the circulation and the Kiwi of skin blood, anti-inflammatory is arranged, prevent and treat effects such as tetter.At present policosanol as the natural health foodstuff additive, in functional food, be applied to candy, beverage, capsule, capsule and pill, tablet, chocolate, cake and biscuit etc.Policosanol is since coming to light, and its exploitation is the focus of current protective foods research and development with research always.
Sugarcane skin in the sugarcane adheres to many cerosins because of the needs of sugarcane production autoprotection, and its staple is a policosanol.Policosanol is attached to the Sugarcane peel. top layer, and after the sugarcane juice of squeezing out, policosanol is just stayed in the bagasse.The method of from sugarcane raw material, extracting at present policosanol mainly is the organic solvent extraction method, with cerosin saponification or transesterify in basic soln, through organic solvent extraction, prepares the high purity alkanol with the method for vacuum distilling or recrystallization.There is complex process in this method, the running time is long, yield is low and shortcoming such as environmental pollution is arranged, and in leaching process, consumes a large amount of solvents.Also have and utilize supercritical co from bagasse or sugarcane skin, to extract the report of policosanol, but its extraction time is long, energy consumption is big.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the method for policosanol in a kind of ultrasound-enhanced supercritical carbon dioxide abstraction bagasse is provided.
The present invention realizes through following technical scheme:
The method of policosanol in a kind of ultrasound-enhanced supercritical carbon dioxide abstraction bagasse comprises the steps and processing condition:
A kind of method that extracts policosanol in the bagasse comprises the steps and processing condition:
(1) bagasse powder is broken into powder;
(2) put step (1) gained bagasse powder into extraction kettle, form packing layer;
(3) extraction process: to extraction kettle, feed supercritical co from the bottom, supercritical co sees through the bagasse powder (making the alkanol in the bagasse powder dissolve in supercritical co) of packing layer, flows out extraction kettle from the top, gets into separating still again; In the extraction process supercritical co in the extraction kettle is carried out the UW radiation;
(4) policosanol that dissolves in carbonic acid gas in the separating still is separated, promptly obtained purpose product policosanol.
Preferably, the said ultrasonic frequency of step (3) is 16kHz-24kHz, and power density is 80W/L-120W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 4s/4s-8s/8s.
Preferably, the said ultrasonic frequency of step (4) is 20kHz, and power density is 100W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 6s/6s.
Preferably, it is characterized in that the temperature of the said extraction kettle of step (3) is 35-50 ℃, pressure is 15-35Mpa; The temperature of separating still is 25-35 ℃, and pressure is 0.2-0.5Mpa.
Preferably, the temperature of the said extraction kettle of step (3) is 45 ℃, and pressure is 30Mpa; The temperature of separating still is 30 ℃, and pressure is 0.3Mpa.
Preferably, step (3) 2-4h of said extraction time.
Preferably, the ultrasonic device of the built-in insert of said extraction kettle.
Preferably, the bagasse grinding particle size is the 60-200 order in the said step (1).
Preferably, said bagasse grinding particle size is the 100-150 order.
Preferably, said bagasse passes through sorting, cleaning, sterilization and exsiccant pre-treatment successively before pulverizing.
The present invention has following advantage and beneficial effect:
1, the present invention is with advanced person's the ultrasound-enhanced supercritical Carbon Dioxide Application preparation technology in extraction policosanol from bagasse; Compare with traditional supercritical carbon dioxide extraction method; Ultrasound-enhanced supercritical carbon dioxide abstraction policosanol can significantly improve extraction efficiency; Reduce extracting pressure and temperature, reduce the extraction time.
2, adopt supercritical carbon dioxide extraction, saved precipitation and the technology that reclaims organic solvent, the carbonic acid gas recycle, cost is lower; Can prevent that product is rotten, product is not polluted by organic solvent, its product can safe being used in food, medicine or the makeup.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is a policosanol standard specimen GC color atlas;
Fig. 3 is the policosanol standard specimen GC color atlas of embodiment 3.
Embodiment
Below in conjunction with embodiment the present invention is described further, the scope that the present invention requires to protect is not limited to the scope that embodiment explains.
Embodiment 1
Bagasse adopts kibbler to be ground into powder through sorting, cleaning, sterilization, drying, crosses 200 mesh sieves; With grinding particle size is the extraction kettle that 1 kilogram of bagasse powder of 200 purposes is put the ultrasonic device of built-in insert into, forms packing layer; Supercritical co gets into extraction kettle from the bottom under pressure-driven, see through the bagasse powder of packing layer; Flow out extraction kettle again from the top, get into separating still, extract after 2 hours through reducing valve; Open separating still after the step-down, in open plastics pot, obtain about 55 grams of ointment to product separation; Ultrasonic frequency is 16kHz when wherein extracting, and power density is 80W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 4s/4s; The temperature of extraction kettle is 35 ℃, and pressure is 15Mpa; The temperature of separating still is 25 ℃, and pressure is 0.2Mpa.
Embodiment 2
Bagasse adopts kibbler to be ground into powder through sorting, cleaning, sterilization, drying, crosses 60 mesh sieves; With grinding particle size is the extraction kettle that 1 kilogram of bagasse powder of 60 purposes is put the ultrasonic device of built-in insert into, forms packing layer; Supercritical co gets into extraction kettle from the bottom under pressure-driven, see through the bagasse powder of packing layer; Flow out extraction kettle again from the top, get into separating still, extract after 3 hours through reducing valve; Open separating still after the step-down, in open plastics pot, obtain about 51 grams of ointment to product separation; Wherein said ultrasonic frequency is 24kHz, and power density is 120W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 8s/8s; The temperature of extraction kettle is 50 ℃, and pressure is 35Mpa; The temperature of separating still is 25 ℃, and pressure is 0.5Mpa.
Embodiment 3:
Bagasse adopts kibbler to be ground into powder through sorting, cleaning, sterilization, drying, crosses 100 mesh sieves; With grinding particle size is the extraction kettle that 1 kilogram of bagasse powder of 100 purposes is put the ultrasonic device of built-in insert into, forms packing layer; Supercritical co gets into extraction kettle from the bottom under pressure-driven, see through the bagasse powder of packing layer; Flow out extraction kettle again from the top, get into separating still, extract after 4 hours through reducing valve; Open separating still after the step-down, in open plastics pot, obtain about 62 grams of ointment to product separation; Wherein said ultrasonic frequency is 20kHz, and power density is 100W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 6s/6s; The temperature of extraction kettle is 45 ℃, and pressure is 30Mpa; The temperature of separating still is 30 ℃, and pressure is 0.3Mpa.
Check and analysis:
Adopt the content of above-mentioned 3 the embodiment gained policosanols of gas chromatography determination.
Instrument: the 6890GC/5975MS of Agilent company;
Reagent: the policosanol reference substance is provided by SIGMA company.
Chromatographic condition: HP-5MS elastic quartz capillary column jecket (30m * 0.25mm * 0.25 μ m); 250 ℃ of injector temperatures; Column temperature: 250 ℃; Heating schedule is 160 ℃ of beginning temperature, keeps being raised to 280 ℃ of maintenance 20min with 10 ℃/min behind the 3min.Carrier gas is a high pure nitrogen, flow velocity 1.0mL/min; Sample size 1 μ L.
Table 1 policosanol yield and assay result
Learn through above-mentioned analyzing and testing: the policosanol yield for preparing according to method of the present invention is more than 5%, and content is more than 28%, and extract purity is high, explains that method of the present invention has applications well and is worth.
Claims (10)
1. a method that extracts policosanol in the bagasse is characterized in that, comprises the steps and processing condition:
(1) bagasse powder is broken into powder;
(2) put step (1) gained bagasse powder into extraction kettle, form packing layer;
(3) extraction process: to extraction kettle, feed supercritical co from the bottom, supercritical co sees through the bagasse powder of packing layer, flows out extraction kettle from the top, gets into separating still again; In the extraction process supercritical co in the extraction kettle is carried out the UW radiation;
(4) policosanol that dissolves in carbonic acid gas in the separating still is separated got final product.
2. method according to claim 1 is characterized in that, the said ultrasonic frequency of step (3) is 16kHz-24kHz, and power density is 80W/L-120W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 4s/4s-8s/8s.
3. method according to claim 2 is characterized in that, the said ultrasonic frequency of step (4) is 20kHz, and power density is 100W/L, the ultrasound wave irradiation mode be the quiescent interval/the continuous irradiation time is 6s/6s.
4. according to claim 1 or 2 or 3 described methods, it is characterized in that the temperature of the said extraction kettle of step (3) is 35-50 ℃, pressure is 15-35Mpa.
5. method according to claim 4 is characterized in that, the temperature of the said extraction kettle of step (3) is 45 ℃, and pressure is 30Mpa.
6. method according to claim 5 is characterized in that, step (3) 2-4h of said extraction time.
7. method according to claim 6 is characterized in that, the ultrasonic device of the built-in insert of said extraction kettle.
8. method according to claim 7 is characterized in that, the bagasse grinding particle size is the 60-200 order in the said step (1).
9. method according to claim 8 is characterized in that, said bagasse grinding particle size is the 100-150 order.
10. method according to claim 9 is characterized in that, said bagasse passes through sorting, cleaning, sterilization and exsiccant pre-treatment successively before pulverizing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110362881.8A CN102399129B (en) | 2011-11-16 | 2011-11-16 | Method for extracting 1-octacosanol from bagasse |
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| CN201110362881.8A CN102399129B (en) | 2011-11-16 | 2011-11-16 | Method for extracting 1-octacosanol from bagasse |
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| CN102399129B CN102399129B (en) | 2014-07-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104450377A (en) * | 2014-11-18 | 2015-03-25 | 广西海酩威酿酒有限公司 | Method for producing policosanol-containing rum by using fresh sugar cane juice |
| CN104957602A (en) * | 2015-05-22 | 2015-10-07 | 长沙普源生物科技有限公司 | Sugarcane bioactive component composition, functional health food, and preparation method of sugarcane bioactive component composition and functional health food |
| CN108794689A (en) * | 2018-06-18 | 2018-11-13 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method for the sugarcane alkanol microsphere polymer that silica gel/beta-cyclodextrin is modified |
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2011
- 2011-11-16 CN CN201110362881.8A patent/CN102399129B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 赵健: "从甘蔗制糖副产物中生产对香豆酸和二十八烷醇", 《中国优秀硕士学位论文全文数据库 》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104450377A (en) * | 2014-11-18 | 2015-03-25 | 广西海酩威酿酒有限公司 | Method for producing policosanol-containing rum by using fresh sugar cane juice |
| CN104957602A (en) * | 2015-05-22 | 2015-10-07 | 长沙普源生物科技有限公司 | Sugarcane bioactive component composition, functional health food, and preparation method of sugarcane bioactive component composition and functional health food |
| CN104957602B (en) * | 2015-05-22 | 2018-06-19 | 长沙普源生物科技有限公司 | Sugarcane active component composition and functional health-care food and preparation method thereof |
| CN108794689A (en) * | 2018-06-18 | 2018-11-13 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method for the sugarcane alkanol microsphere polymer that silica gel/beta-cyclodextrin is modified |
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