CN103570788A - Method for purifying beta-sitosterol in blendimiss sterol - Google Patents
Method for purifying beta-sitosterol in blendimiss sterol Download PDFInfo
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- CN103570788A CN103570788A CN201310584677.XA CN201310584677A CN103570788A CN 103570788 A CN103570788 A CN 103570788A CN 201310584677 A CN201310584677 A CN 201310584677A CN 103570788 A CN103570788 A CN 103570788A
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Abstract
A method for purifying beta-sitosterol in blendimiss sterol comprises the following steps: (1), under a condition of 65 to 75 DEG C, using ethyl alcohol for heat dissolution to the blendimiss sterol, filtering, infiltrating a filter liquor into a cold crystallization kettle, lowering the temperature to 5 to 10 DEG C, using a plate-and-frame filter press for filtering; (2), throwing a filter cake obtained in the step 1 and ethyl alcohol into a reaction kettle, and after 1 to 2 hours stirring, using the plate-and-frame filter press for filtering; (3), adding the filter cake obtained in the step 2 and the cyclohexanone into the reaction kettle, increasing the temperature to 55 plus or minus 2 DGE C, after stirring for 20 to 40 minutes at a constant temperature, reducing the temperature to 25 to 30 DEG C, and using the plate-and-frame filter press for filtering; (4), adding the filter cake obtained in the step 3 and cyclohexanone into the reaction kettle, increasing the temperature to 55 plus or minus 2 DGE C, after stirring for 20 to 40 minutes at a constant temperature, reducing the temperature to 25 to 30 DEG C, and filtering at a constant temperature; (5), repeating the step (4) to obtain a filter cake and placing the filter cake in a vacuum drying machine, and carrying out vacuum drying under a condition of 60 plus or minus 2 DEG C. The method provided by the invention is simple in process, convenient to operate, low in cost, high in product yield and high in purity.
Description
Technical field
The present invention relates to a kind of method of the β-sitosterol in mixed phytosterin of purifying.
Background technology
β-sitosterol is a kind of of plant sterol, belongs to steroidal compounds, is present in vegetables oil and oleaginous food.Grease is (as alkali refining, decolouring, deodorizing) after refining, and sterol mainly concentrates in the distillation leftover of oil alkali refining soap stock, deodorization distillate, lipid acid and ester, thereby becomes the main raw material(s) that sterol extracts.β-sitosterol has the effect of the cholesterol of reduction; Anti-inflammatory, bring down a fever, antiulcer action; Antitumor action, medicine, makeup, food, etc. field have extensive use, there are good market outlook.In recent years plant sterol on medicine industry further application its purity is proposed to requirements at the higher level, how mixed phytosterin is separated into single sterol product, and improves its yield and purity becomes main technical bottleneck at present.
The separation method existing at present mainly contains chemical method, chromatography, crystallization process etc.
Chemical method is mainly to utilize chemical reaction to prepare the derivative of plant sterol, increases the physical difference of each plant sterols, and recycling Physical is separated.Chinese patent CN1583780A discloses a kind of method of preparing high-content beta-sitosterin products by catalytic hydrogenation, by mixed phytosterin raw material, be dissolved in the middle of organic solvent, under the condition of normal temperature and pressure or pressurization, make spent hydroprocessing catalyst carry out catalytic hydrogenation, Stigmasterol in mixed phytosterin is generated to β-sitosterol with addition of hydrogen, finally obtain the β-sitosterol of liquid high-content, the content range of β-sitosterol is 60-75%.Chemical process yield is better, but in scale operation, exists reactions steps many, and cost is high, operational difficulty, the shortcoming such as environmental pollution is large, and solvent recovering rate is low.
Chromatography is to utilize the difference of the adsorption/desorption power of each component of plant sterol in chromatogram filling liquid and the asynchronism(-nization) of flowing out chromatographic column, reaches the object of purification.Chinese patent CN101367860A disclose a kind of from mixed phytosterin the method for separating and extracting beta-sitosterol, mixed plant β-sitosterol is dissolved in organic solvent, through metal-chelate resin, adsorb, each component in mixture is selectively adsorbed on metal-chelate resin, metal-chelate resin is again through eluent wash-out β-sitosterol, realize the separation of β-sitosterol in mixed phytosterin, metal-chelate resin, after manipulation of regeneration, is reused.Although aforesaid method DNA purity is high, equipment cost is too large, realizes scale operation more difficult.
Crystallization process is to utilize indivedual sterols dissolubility difference in solvent to carry out multistep fractional crystallization, though crystallization number of times is more, technique is simple, easy to operate, and purity is higher, is applicable to batch production and produces.At present, about mixing sterol monomer separation study general, be to adopt solvent crystallization both at home and abroad, still, because the solvability difference between each component of plant sterol is less, thereby to select suitable solvent and operational condition be to realize effectively separated bottleneck.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of cost low, the method for the β-sitosterol in the high purification mixed phytosterin of product yield and purity.
The technical solution adopted for the present invention to solve the technical problems: a kind of method of the β-sitosterol in mixed phytosterin of purifying, comprises the following steps:
(1) under the condition of temperature 65-70 ℃, with mixed phytosterin quality 6-8 doubly alcohol mixed phytosterin is carried out to heat of solution, the solution filter after heat of solution is removed to impurity, filtrate after filtering is squeezed into cold analysis still, be cooled to after 5-10 ℃, with plate-and-frame filter press, filter, obtain filter cake;
(2) ratio that is 3-5:1 in the mass ratio of step (1) gained filter cake and alcohol, drops into reactor by filter cake and alcohol, stirs after 1-2h, then filters with plate-and-frame filter press, obtains filter cake;
(3) ratio that is 1:3-5 in the mass ratio of step (2) gained filter cake and pimelinketone, adds reactor by filter cake and pimelinketone, is then warming up to 2 ℃ of 55 scholars, and constant temperature stirred after 20-40 minute, was cooled to 25-30 ℃, with flame filter press, filters, and obtains filter cake;
(4) ratio that is 1:3-5 in the mass ratio of step (3) gained filter cake and pimelinketone, adds reactor by filter cake and pimelinketone, is then warming up to 2 ℃ of 55 scholars, and constant temperature stirred after 20-40 minute, was cooled to 25-30 ℃, temperature filtration;
(5) repeating step (4), until the mass content of β-sitosterol reaches more than 90% in filter cake, then puts into Vacuumdrier by filter cake, vacuum-drying under 2 ℃ of conditions of temperature 60 scholar.
Further, in step (1), in described mixed phytosterin, total sterol mass content is 50 scholars 10%.
Further, in step (1), the volume fraction of described alcohol is 90-99%(preferably 95%).
Further, in step (2), the volume fraction of described alcohol is 90-99%(preferably 95%).
Further, in step (3), volume fraction >=95% of described pimelinketone.
Further, in step (4), volume fraction >=95% of described pimelinketone.
The present invention adopts solvent crystallization, selecting by volume fraction is 90-99%(preferably 95%) alcohol as purification solvent, pimelinketone is as fractional crystallization solvent, compare with existing other solvent method, the present invention is easy and simple to handle, and solvent recuperation is easy, product yield high (more than 70%), purity high (more than 90%), cost is low.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1
The present embodiment comprises the following steps:
(1) under the condition of temperature 70 C, the alcohol that is 95% by the volume fraction of 7 times of mixed phytosterin quality carries out heat of solution to mixed phytosterin (total sterol mass content is 55%), solution filter after heat of solution is removed to impurity, filtrate after filtering is squeezed into cold analysis still, be cooled to after 10 ℃, with plate-and-frame filter press, filter, obtain filter cake;
(2) ratio that the mass ratio of the alcohol that is 95% in step (1) gained filter cake and volume fraction is 3:1, filter cake and alcohol are dropped into reactor, stir after 1h, then filter with plate-and-frame filter press, obtain filter cake, the mixed phytosterin mass content in gained filter cake reaches 92.7%;
(3) ratio that is 1:4 in the mass ratio of step (2) gained filter cake and pimelinketone (volume fraction 95%), adds reactor by filter cake and pimelinketone, is then warming up to 55 ℃, constant temperature stirred after 40 minutes, be cooled to 30 ℃, with flame filter press, filter, obtain filter cake;
(4) ratio that is 1:4 in the mass ratio of step (3) gained filter cake and pimelinketone (volume fraction 95%), adds reactor by filter cake and pimelinketone, is then warming up to 55 ℃, and constant temperature stirred after 40 minutes, was cooled to 30 ℃, temperature filtration;
(5) repeating step (4), obtains filter cake, then filter cake is put into Vacuumdrier, and vacuum-drying under 62 ℃ of conditions of temperature, then pulverizes and sieves, and is packed as finished product; The mass content that records β-sitosterol reaches 94.3%, and yield is 70.6%.
embodiment 2
The present embodiment comprises the following steps:
(1) under the condition of 67 ℃ of temperature, the alcohol that is 95% by the volume fraction of 7 times of mixed phytosterin quality carries out heat of solution to mixed phytosterin (total sterol mass content is 50%), solution filter after heat of solution is removed to impurity, filtrate after filtering is squeezed into cold analysis still, be cooled to after 10 ℃, with plate-and-frame filter press, filter, obtain filter cake;
(2) ratio that the mass ratio of the alcohol that is 95% in step (1) gained filter cake and volume fraction is 3:1, filter cake and alcohol are dropped into reactor, stir after 1.5h, then filter with plate-and-frame filter press, obtain filter cake, the mixed phytosterin mass content in gained filter cake reaches 93.5%;
(3) ratio that is 1:5 in the mass ratio of step (2) gained filter cake and pimelinketone (volume fraction 95%), adds reactor by filter cake and pimelinketone, is then warming up to 52 ℃, constant temperature stirred after 30 minutes, be cooled to 25 ℃, with flame filter press, filter, obtain filter cake;
(4) ratio that is 1:5 in the mass ratio of step (3) gained filter cake and pimelinketone (volume fraction 95%), adds reactor by filter cake and pimelinketone, is then warming up to 52 ℃, and constant temperature stirred after 30 minutes, was cooled to 25 ℃, temperature filtration;
(5) repeating step (4), obtains filter cake, then filter cake is put into Vacuumdrier, and vacuum-drying under temperature 60 C condition, then pulverizes and sieves, and is packed as finished product; The mass content that records β-sitosterol reaches 92.4%, and yield is 71.5%.
Claims (6)
1. the purify method of the β-sitosterol in mixed phytosterin, is characterized in that, comprises the following steps:
(1) under the condition of temperature 65-70 ℃, with mixed phytosterin quality 6-8 alcohol doubly, mixed phytosterin is carried out to heat of solution, the solution filter after heat of solution is removed to impurity, filtrate after filtering is squeezed into cold analysis still, be cooled to after 5-10 ℃, with plate-and-frame filter press, filter, obtain filter cake;
(2) ratio that is 3-5:1 in the mass ratio of step (1) gained filter cake and alcohol, drops into reactor by filter cake and alcohol, stirs after 1-2h, then filters with plate-and-frame filter press, obtains filter cake;
(3) ratio that is 1:3-5 in the mass ratio of step (2) gained filter cake and pimelinketone, adds reactor by filter cake and pimelinketone, is then warming up to 2 ℃ of 55 scholars, and constant temperature stirred after 20-40 minute, was cooled to 25-30 ℃, with flame filter press, filters, and obtains filter cake;
(4) ratio that is 1:3-5 in the mass ratio of step (3) gained filter cake and pimelinketone, adds reactor by filter cake and pimelinketone, is then warming up to 2 ℃ of 55 scholars, and constant temperature stirred after 20-40 minute, was cooled to 25-30 ℃, temperature filtration;
(5) repeating step (4), until the mass content of β-sitosterol reaches more than 90% in filter cake, then puts into Vacuumdrier by filter cake, vacuum-drying under 2 ℃ of conditions of temperature 60 scholar.
2. the method for the β-sitosterol in purification mixed phytosterin according to claim 1, is characterized in that, in step (1), in described mixed phytosterin, total sterol mass content is 50 scholars 10%.
3. the method for the β-sitosterol in purification mixed phytosterin according to claim 1 and 2, is characterized in that, in step (1), the volume fraction of described alcohol is 90-99%.
4. the method for the β-sitosterol in purification mixed phytosterin according to claim 1 and 2, is characterized in that, in step (2), the volume fraction of described alcohol is 90-99%.
5. the method for the β-sitosterol in purification mixed phytosterin according to claim 1 and 2, is characterized in that, in step (3), and volume fraction >=95% of described pimelinketone.
6. the method for the β-sitosterol in purification mixed phytosterin according to claim 1 and 2, is characterized in that, in step (4), and volume fraction >=95% of described pimelinketone.
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| CN201310584677.XA CN103570788A (en) | 2013-11-20 | 2013-11-20 | Method for purifying beta-sitosterol in blendimiss sterol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111171099A (en) * | 2020-01-17 | 2020-05-19 | 杭州益品新五丰药业有限公司 | Method for extracting sitosterol by double-solvent crystallization and sitosterol extracted by using method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544676A (en) * | 2009-05-06 | 2009-09-30 | 陕西天维生物制品有限责任公司 | Method of extracting beta-sitosterol from n-pentanol solvent crystallization |
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- 2013-11-20 CN CN201310584677.XA patent/CN103570788A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544676A (en) * | 2009-05-06 | 2009-09-30 | 陕西天维生物制品有限责任公司 | Method of extracting beta-sitosterol from n-pentanol solvent crystallization |
Non-Patent Citations (1)
| Title |
|---|
| 许文林等: "结晶法分离精制混合植物甾醇中β-谷甾醇和豆甾醇", 《过程工程学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111171099A (en) * | 2020-01-17 | 2020-05-19 | 杭州益品新五丰药业有限公司 | Method for extracting sitosterol by double-solvent crystallization and sitosterol extracted by using method |
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Application publication date: 20140212 |