CN101544676A - Method of extracting beta-sitosterol from n-pentanol solvent crystallization - Google Patents
Method of extracting beta-sitosterol from n-pentanol solvent crystallization Download PDFInfo
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- CN101544676A CN101544676A CN200910022376A CN200910022376A CN101544676A CN 101544676 A CN101544676 A CN 101544676A CN 200910022376 A CN200910022376 A CN 200910022376A CN 200910022376 A CN200910022376 A CN 200910022376A CN 101544676 A CN101544676 A CN 101544676A
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Abstract
The invention discloses a method of extracting beta-sitosterol from n-pentanol solvent crystallization. Under certain temperature, alcohol of 95 percent with 7 times the amount of crude sterols is used to carry out thermal dissolution on the crude sterols; impurities are filtered through micropores; filter liquor is pumped into a cold separation reactor be filtered after being cooled to 10 DEG C; a filter cake and the alcohol are added into a reactor according to the mass ratio of 3 : 1, fully mixed and filtered; n-pentanol and the filter cake with the mass ratio of 3 to 5 : 1 are added into the reactor, temperature then rises to 40 DEGC plus/minus 2 DEG C, and the n-pentanol and the filter cake are fully mixed keeping the temperature unchanged; the steps are repeated to ensure that content of the beta-sitosterol in the filter cake achieves above 90 percent, and then the filter cake is dried in vacuum, crashed, sieved and packaged into a finished product. Compared with other solvent methods, the invention has high product yield and low cost. Solvent mixture is used in other solvent methods, while the invention uses single solvent n-pentanol having easy recovery and simple operation.
Description
Technical field
The present invention relates to a kind of extracting method of β-Gu Zaichun, be specifically related to the method that a kind of Pentyl alcohol solvent crystallization extracts β-Gu Zaichun.
Background technology
β-Gu Zaichun is a kind of of plant sterol, belongs to steroidal compounds, has stronger anti-inflammatory and antiinflammation, and has the antipyretic effect of similar acetylsalicylic acid (acetylsalicylic acid) concurrently; Show that by the long term studies experiment β-Gu Zaichun can suppress chemical carcinogens and bring out large bowel cancer; As everyone knows, plant sterol can effectively reduce serum cholesterol level, play the effect of prevention and cardiovascular disordeies such as treatment hypertension, coronary heart disease, studies show that recently, the selectivity of performance output when β-Gu Zaichun hinders cholesterol absorption, when being lower than 100mg, cholesterol intake demonstrates stopping effect hardly, but if when reaching 400～450mg, even only absorb a spot of β-Gu Zaichun, also can play the effect that reduces the cholesterol in serum level, to the also almost not influence of drainage of bile acide; It is the main the most frequently used starting raw material etc. of producing steroid drugs key intermediate 4AD or ADD.In recent years, the oleomargarine of β-Gu Zaichun has appearred containing in Europe, through authoritative medical journal evaluation, possesses the effect of falling total cholesterol and low density lipoprotein cholesterol.The demand of high-content β-Gu Zaichun heightens.In the plant sterol in the market only there being about 45% the content of β-Gu Zaichun, the highlyest is no more than 65%, and the high-content β-Gu Zaichun still is a blank, and market outlook are wide, and added value is very high.
At present β-Gu Zaichun preparation method mainly contain:
1. chemical method: utilize chemical reaction to prepare the derivative of plant sterol, increase the physical difference of each plant sterols, utilize the physics method to separate again.Usually utilize the difference of the tetrabromide solubleness of the dibromide of β-Gu Zaichun ethyl ester and Stigmasterol ethyl ester, at first mixed phytosterin is carried out esterification with diacetyl oxide, then esterification products is carried out bromination with excessive bromine, select for use suitable separated from solvent to go out dibromide and tetrabromide.Product after the separation is used zinc powder reduction debrominate, alkaline hydrolysis respectively, and recrystallization obtains pure β-Gu Zaichun in acetone at last.
2. physics method: solvent crystallization can directly be separated the mixing sterol, operates comparatively easy.Solvent for use mainly contains: methanol, Virahol, acetoneand ethyl acetate etc.
3. chromatogram preparation method: utilize the difference of the adsorption/desorption power of each component of plant sterol in the chromatogram filling liquid and flow out the asynchronism(-nization) of chromatographic column, reach the purpose of purification.
There are shortcomings such as reactions steps is many, cost is high, operational difficulty, environmental pollution is big, solvent recovering rate is low in aforesaid method 1 in scale operation.Aforesaid method 2 has the short solvent of technical process easy and simple to handle and easily reclaims advantages such as environmental pollution is little, but because the solvability difference between each component of plant sterol is less thereby to select suitable solvent and operational condition be to realize effective isolating bottleneck.Though aforesaid method 3 dna purity height, equipment cost is too big, realizes that scale operation is difficult.
Summary of the invention
The objective of the invention is in order to overcome the deficiencies in the prior art, provide a kind of Pentyl alcohol solvent crystallization to extract the method for β-Gu Zaichun.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of Pentyl alcohol solvent crystallization extracts the method for β-Gu Zaichun, it is characterized in that this procedure is:
(1) under the condition of 70 ℃ of temperature, is that 50% ± 5% thick sterol carries out heat of solution with the alcohol of 7 times of thick sterol quality to the mixed phytosterin mass content, solution after the heat of solution is removed impurity by millipore filtration, filtrate filtered is squeezed into the cold analysis still, after being cooled to 10 ℃ with plate-and-frame filter press filter filter cake, the volumetric concentration of described alcohol is 95%;
(2) press filter cake: the mass ratio of alcohol=3: 1 drops into reactor with filter cake in the step (1) and alcohol, filter with plate-and-frame filter press again after fully stirring, the mixed phytosterin mass content of filtering in the gained filter cake of back reaches more than 90%, and the volumetric concentration of described alcohol is 95%;
(3) press Pentyl alcohol: filter cake=3～5: 1 mass ratio is warming up to 40 ℃ ± 2 ℃ then with gained filter cake in the step (2) and Pentyl alcohol adding reactor, keeps temperature-resistant, fully stirred 20-40 minute, then with flame filter press filter filter cake;
(4) press Pentyl alcohol: filter cake=3～5: 1 mass ratio adds reactor with gained filter cake in the step (3) and Pentyl alcohol, is warming up to 40 ℃ ± 2 ℃ and fully stirs 20-40 minute after-filtration;
(5) repeating step (4) makes that the mass content of β-Gu Zaichun reaches more than 90% in the filter cake, then filter cake is put into Vacuumdrier, vacuum-drying under 60 ℃ ± 2 ℃ conditions of temperature, and crushing screening is packed as finished product then.
The volumetric concentration of Pentyl alcohol is more than 95% described in above-mentioned steps (3) and the step (4).
The mass ratio of Pentyl alcohol and filter cake is 4.2: 1 described in above-mentioned steps (3) and the step (4).
The present invention adopts the solvent crystallization in the physics method, because we have found the solvent Pentyl alcohol of highly selective, and by continuous experimental study, has found suitable operational condition.We discover, the main ingredient β-Gu Zaichun of plant sterol and Stigmasterol are in 30 ℃, solubleness is along with the rising of temperature all slowly raises, but more than 30 ℃, the solubleness of Stigmasterol is along with the rising of temperature continues slowly to raise, and the solubleness of β-Gu Zaichun raises and culminates at 40 ℃ along with the rising of temperature is rapid.Therefore we adopt the Pentyl alcohol saturated solution at 40 ℃ of preparation β-Gu Zaichuns, and at 40 ℃ of temperature filtrations, so repeat 5-6 operation.
The present invention compared with prior art has the following advantages: the present invention is higher by 30% than using other solvent method product yield, cost low 20%; Be to use mixed solvent in other solvent method and the inventive method use single solvent Pentyl alcohol, it is easy to reclaim, simple to operate; The β-Gu Zaichun mass content that the present invention extracts reaches more than 90%.
Below by embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
(1) under the condition of 70 ℃ of temperature, is that 50% thick sterol carries out heat of solution with the alcohol of 7 times of thick sterol quality to the mixed phytosterin mass content, solution after the heat of solution is removed impurity by millipore filtration, filtrate filtered is squeezed into the cold analysis still, after being cooled to 10 ℃ with plate-and-frame filter press filter filter cake, the volumetric concentration of described alcohol is 95%;
(2) press filter cake: the mass ratio of alcohol=3: 1 drops into reactor with filter cake in the step (1) and alcohol, filter with plate-and-frame filter press again after fully stirring, the mixed phytosterin mass content of filtering in the gained filter cake of back reaches more than 90%, and the volumetric concentration of described alcohol is 95%;
(3) press Pentyl alcohol: the mass ratio of filter cake=4.2: 1 is with gained filter cake in the step (2) and Pentyl alcohol adding reactor, be warming up to 40 ℃ then, keep temperature-resistant, fully stirred 30 minutes, then with flame filter press filter filter cake, the volumetric concentration of described Pentyl alcohol is more than 95%;
(4) press Pentyl alcohol: the mass ratio of filter cake=4.2: 1 adds reactor with gained filter cake in the step (3) and Pentyl alcohol, is warming up to 40 ℃ of fully 30 minutes after-filtration of stirring, and the volumetric concentration of described Pentyl alcohol is more than 95%;
(5) repeating step (4) makes that the mass content of β-Gu Zaichun reaches more than 90% in the filter cake, then filter cake is put into Vacuumdrier, vacuum-drying under 60 ℃ of conditions of temperature, and crushing screening is packed as finished product then.
Embodiment 2
(1) under the condition of 70 ℃ of temperature, is that 55% thick sterol carries out heat of solution with the alcohol of 7 times of thick sterol quality to the mixed phytosterin mass content, solution after the heat of solution is removed impurity by millipore filtration, filtrate filtered is squeezed into the cold analysis still, after being cooled to 10 ℃ with plate-and-frame filter press filter filter cake, the volumetric concentration of described alcohol is 95%;
(2) press filter cake: the mass ratio of alcohol=3: 1 drops into reactor with filter cake in the step (1) and alcohol, filter with plate-and-frame filter press again after fully stirring, the mixed phytosterin mass content of filtering in the gained filter cake of back reaches more than 90%, and the volumetric concentration of described alcohol is 95%;
(3) press Pentyl alcohol: the mass ratio of filter cake=5: 1 is with gained filter cake in the step (2) and Pentyl alcohol adding reactor, be warming up to 42 ℃ then, keep temperature-resistant, fully stirred 40 minutes, then with flame filter press filter filter cake, the volumetric concentration of described Pentyl alcohol is more than 95%;
(4) press Pentyl alcohol: the mass ratio of filter cake=5: 1 adds reactor with gained filter cake in the step (3) and Pentyl alcohol, is warming up to 42 ℃ of fully 40 minutes after-filtration of stirring, and the volumetric concentration of described Pentyl alcohol is more than 95%;
(5) repeating step (4) makes that the mass content of β-Gu Zaichun reaches more than 90% in the filter cake, then filter cake is put into Vacuumdrier, vacuum-drying under 62 ℃ of conditions of temperature, and crushing screening is packed as finished product then.
Embodiment 3
(1) under the condition of 70 ℃ of temperature, is that 45% thick sterol carries out heat of solution with the alcohol of 7 times of thick sterol quality to the mixed phytosterin mass content, solution after the heat of solution is removed impurity by millipore filtration, filtrate filtered is squeezed into the cold analysis still, after being cooled to 10 ℃ with plate-and-frame filter press filter filter cake, the volumetric concentration of described alcohol is 95%;
(2) press filter cake: the mass ratio of alcohol=3: 1 drops into reactor with filter cake in the step (1) and alcohol, filter with plate-and-frame filter press again after fully stirring, the mixed phytosterin mass content of filtering in the gained filter cake of back reaches more than 90%, and the volumetric concentration of described alcohol is 95%;
(3) press Pentyl alcohol: the mass ratio of filter cake=3: 1 is with gained filter cake in the step (2) and Pentyl alcohol adding reactor, be warming up to 38 ℃ then, keep temperature-resistant, fully stirred 20 minutes, then with flame filter press filter filter cake, the volumetric concentration of described Pentyl alcohol is more than 95%;
(4) press Pentyl alcohol: the mass ratio of filter cake=3: 1 adds reactor with gained filter cake in the step (3) and Pentyl alcohol, is warming up to 38 ℃ of fully 20 minutes after-filtration of stirring, and the volumetric concentration of described Pentyl alcohol is more than 95%;
(5) repeating step (4) makes that the mass content of β-Gu Zaichun reaches more than 90% in the filter cake, then filter cake is put into Vacuumdrier, vacuum-drying under 58 ℃ of conditions of temperature, and crushing screening is packed as finished product then.
Product the key technical indexes such as following table that the present invention extracts:
| Project | Outward appearance | Heavy metal | Arsenic | Total sterol |
| Index | White powder | ≤10ppm | ≤1ppm | >95％ |
| Project | β-Gu Zaichun | Stigmasterol | Campesterol | Brassicasterol |
| Index | ≥90％ | ≤1.0％ | ≤8.0％ | ≤1.0％ |
Claims (3)
1. a Pentyl alcohol solvent crystallization extracts the method for β-Gu Zaichun, it is characterized in that this procedure is:
(1) under the condition of 70 ℃ of temperature, is that 50% ± 5% thick sterol carries out heat of solution with the alcohol of 7 times of thick sterol quality to the mixed phytosterin mass content, solution after the heat of solution is removed impurity by millipore filtration, filtrate filtered is squeezed into the cold analysis still, after being cooled to 10 ℃ with plate-and-frame filter press filter filter cake, the volumetric concentration of described alcohol is 95%;
(2) press filter cake: the mass ratio of alcohol=3: 1 drops into reactor with filter cake in the step (1) and alcohol, filter with plate-and-frame filter press again after fully stirring, the mixed phytosterin mass content of filtering in the gained filter cake of back reaches more than 90%, and the volumetric concentration of described alcohol is 95%;
(3) press Pentyl alcohol: filter cake=3～5: 1 mass ratio is warming up to 40 ℃ ± 2 ℃ then with gained filter cake in the step (2) and Pentyl alcohol adding reactor, keeps temperature-resistant, fully stirred 20-40 minute, then with flame filter press filter filter cake;
(4) press Pentyl alcohol: filter cake=3～5: 1 mass ratio adds reactor with gained filter cake in the step (3) and Pentyl alcohol, is warming up to 40 ℃ ± 2 ℃ and fully stirs 20-40 minute after-filtration;
(5) repeating step (4) makes that the mass content of β-Gu Zaichun reaches more than 90% in the filter cake, then filter cake is put into Vacuumdrier, vacuum-drying under 60 ℃ ± 2 ℃ conditions of temperature, and crushing screening is packed as finished product then.
2. Pentyl alcohol solvent crystallization according to claim 1 extracts the method for β-Gu Zaichun, it is characterized in that the volumetric concentration of Pentyl alcohol described in step (3) and the step (4) is more than 95%.
3. Pentyl alcohol solvent crystallization according to claim 1 extracts the method for β-Gu Zaichun, it is characterized in that the mass ratio of Pentyl alcohol described in step (3) and the step (4) and filter cake is 4.2: 1.
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| CN200910022376A CN101544676A (en) | 2009-05-06 | 2009-05-06 | Method of extracting beta-sitosterol from n-pentanol solvent crystallization |
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| CN200910022376A CN101544676A (en) | 2009-05-06 | 2009-05-06 | Method of extracting beta-sitosterol from n-pentanol solvent crystallization |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570788A (en) * | 2013-11-20 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for purifying beta-sitosterol in blendimiss sterol |
| CN103570786A (en) * | 2013-11-20 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for segmented purification of beta-sitosterol and stigmasterol by using n-amyl alcohol |
| CN103570787A (en) * | 2013-11-20 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for separating beta-sitosterol and stigmasterol from mixed phytosterol |
| 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 |
-
2009
- 2009-05-06 CN CN200910022376A patent/CN101544676A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570788A (en) * | 2013-11-20 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for purifying beta-sitosterol in blendimiss sterol |
| CN103570786A (en) * | 2013-11-20 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for segmented purification of beta-sitosterol and stigmasterol by using n-amyl alcohol |
| CN103570787A (en) * | 2013-11-20 | 2014-02-12 | 湖南科源生物制品有限公司 | Method for separating beta-sitosterol and stigmasterol from mixed phytosterol |
| CN103570787B (en) * | 2013-11-20 | 2017-01-04 | 湖南科源生物制品有限公司 | A kind of separation cupreol and method of stigmasterol from mixed phytosterin |
| CN103570786B (en) * | 2013-11-20 | 2017-01-04 | 湖南科源生物制品有限公司 | A kind of n-amyl alcohol segmentation purifies cupreol and the method for stigmasterol |
| 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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Open date: 20090930 |