CN103183705A - Method for preparing high purity cephalin - Google Patents
Method for preparing high purity cephalin Download PDFInfo
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- CN103183705A CN103183705A CN 201110446654 CN201110446654A CN103183705A CN 103183705 A CN103183705 A CN 103183705A CN 201110446654 CN201110446654 CN 201110446654 CN 201110446654 A CN201110446654 A CN 201110446654A CN 103183705 A CN103183705 A CN 103183705A
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Abstract
The invention discloses a method for preparing high purity cephalin, which comprises the steps of: first centrifuging rapeseed oil residue, drying precipitate in a vacuum oven, adding acetone to dehydrated rapeseed oil residue and mixing, removing upper oil-containing acetone after standing, operating as the above methods for 2-3 times to thoroughly remove oil in the rapeseed oil residue, drying in vacuum to get powder phosphatide, mixing the power phosphatide and 95% ethanol, putting on a constant temperature heating magnetic mixer, stirring for extraction, separating, dissolving alcohol insoluble substances in ether, precipitating with acetone, drying the precipitate in vacuum to get crude PE, separating the raw material of the rough PE by a column chromatograph, wherein chromatography silica gel is activated in an oven for 60 minutes before packing in the column and a small amount of chloroform-methanol is used as an eluent, and drying and concentrating the PE product in vacuum to get high purity PE. The technical solution of the invention is good in separation effect and high in product quality.
Description
Technical field
The present invention relates to phosphorus compound, particularly relate to a kind of method for preparing the high purity kephalin.
Background technology
China's Semen Brassicae campestris aboundresources, the annual rapeseed oil residue that produces up to ten thousand tons, rapeseed oil residue such as untimely processing treatment are very easily become sour smelly and can't be used, and contaminate environment.Mostly the utilization of existing rapeseed oil residue is to make acidifying oil, has ignored higher this advantage of phospholipids content in the rapeseed oil residue, causes the waste of phosphatide resource.
Vegetable seed phosphatide is a kind of mixture, and its main component is Yelkin TTS (PC), kephalin (PE), serine phosphatide (PS), lipositol (PI) etc.According to the literature, kephalin content in the vegetable seed phosphatide is a little more than in the soybean phospholipid, so as the raw material of kephalin preparation, vegetable seed phosphatide has more advantage than soybean phospholipid.
The branch extracting method of vegetable seed phosphatide has much at present, divides formulation, high performance liquid chromatography, column chromatography, tlc, acetylation method, enzyme process etc. as the inorganic salt precipitator method, solvent.But wherein some method such as acetylation method can only extract Yelkin TTS, and high performance liquid chromatography and tlc, preparation amount is less, is not suitable for industrial production.
By retrieval, also there is not the solvent branch put forward with column chromatography to combine the processing method of the high-purity kephalin of preparation from rapeseed oil residue in the Chinese patent storehouse.
Summary of the invention
The purpose of this invention is to provide a kind of good separating effect, be fit to the industrial method for preparing the high purity kephalin.
Realize that technical scheme of the present invention is to carry out according to the following steps:
(1) earlier with the rapeseed oil residue centrifugation, the throw out of gained is dry in vacuum drying oven, carries out vacuum hydro-extraction;
(2) rapeseed oil residue after the dehydration adds a certain amount of acetone and mixes and stir, and makes that contained oil is dissolved in acetone in the rapeseed oil residue, removes upper strata oil-containing acetone after leaving standstill; Institute's oil-containing in the rapeseed oil residue is thoroughly removed in aforesaid method operation 2～3 times, and vacuum-drying subsequently namely gets powder lecithin;
(3) gained powder lecithin and 95% ethanol are mixed, put into the thermostatically heating magnetic stirring apparatus, stirring and leaching is separated then, and the gained alcohol insoluble solids is earlier through ether dissolution, and back acetone precipitation, throw out get thick PE after vacuum-drying;
(4) be raw material with thick PE, carrying out column chromatography in chromatographic column separates, silica gel for chromatography dress post is prepended in 120 ℃ of baking ovens and activates 60 minutes, is eluent with small amounts of chlorine imitation-carbinol (volume ratio is 2: 1), and gained PE product obtains high-purity PE after the vacuum concentration drying.
The temperature control of above-mentioned vacuum drying oven is at 55～63 ℃.
The above-mentioned vacuum drying time is 10～15 hours.
The flow velocity of above-mentioned eluent is 3mL/ minute.
The invention has the beneficial effects as follows: (1) method of the present invention is carried the solvent branch with column chromatography and is combined, and effectively avoided the relatively poor problem of independent employing solvent branch formulation separating effect, and cost is lower; Have also that column chromatography equipment is simple, the advantage of good separating effect; (2) the inventive method can not only obtain high-purity PE product efficiently, and compares with other separation methods, and good separating effect is arranged, the quality product height, and advantage such as disengaging time is short, and solvent consumption is few, high-purity PE lays the first stone for suitability for industrialized production.
Embodiment
Embodiment 1
Earlier with the rapeseed oil residue centrifugation, the throw out of gained is dry in vacuum drying oven, true temperature control is at 58 ℃, dry 10 hours, carry out vacuum hydro-extraction, rapeseed oil residue after the dehydration adds a certain amount of acetone and mixes and stir, and makes that contained oil is dissolved in acetone in the rapeseed oil residue, removes upper strata oil-containing acetone after leaving standstill; Aforesaid method operation 2 times, thoroughly remove institute's oil-containing in the rapeseed oil residue, vacuum-drying subsequently, namely get powder lecithin, gained powder lecithin and 95% ethanol are mixed, put into the thermostatically heating magnetic stirring apparatus, stirring and leaching, separate then, the gained alcohol insoluble solids is first through ether dissolution, the back acetone precipitation, throw out gets thick PE through 60 ℃ of dryings of vacuum after 10 hours, be raw material with thick PE, carry out column chromatography in chromatographic column and separate that silica gel for chromatography dress post was prepended in 120 ℃ of baking ovens activation 60 minutes, be eluent with small amounts of chlorine imitation-carbinol (volume ratio is 2: 1), the flow velocity of control eluent is 3mL/ minute, and gained PE product obtains high-purity PE after the vacuum concentration drying, and its purity is 91.4%.
Embodiment 2
Earlier with the rapeseed oil residue centrifugation, the throw out of gained is dry in vacuum drying oven, true temperature control is at 63 ℃, dry 15 hours, carry out vacuum hydro-extraction, rapeseed oil residue after the dehydration adds a certain amount of acetone and mixes and stir, and makes that contained oil is dissolved in acetone in the rapeseed oil residue, removes upper strata oil-containing acetone after leaving standstill; Aforesaid method operation 3 times, thoroughly remove institute's oil-containing in the rapeseed oil residue, vacuum-drying subsequently, namely get powder lecithin, gained powder lecithin and 95% ethanol are mixed, put into the thermostatically heating magnetic stirring apparatus, stirring and leaching, separate then, the gained alcohol insoluble solids is first through ether dissolution, the back acetone precipitation, throw out gets thick PE through 60 ℃ of dryings of vacuum after 12 hours, be raw material with thick PE, carry out column chromatography in chromatographic column and separate that silica gel for chromatography dress post was prepended in 120 ℃ of baking ovens activation 60 minutes, be eluent with small amounts of chlorine imitation-carbinol (volume ratio is 2: 1), the flow velocity of control eluent is 3mL/ minute, and gained PE product obtains high-purity PE after the vacuum concentration drying, and its purity is 94.5%.
Embodiment 3
Earlier with the rapeseed oil residue centrifugation, the throw out of gained is dry in vacuum drying oven, true temperature control is at 55 ℃, dry 12 hours, carry out vacuum hydro-extraction, rapeseed oil residue after the dehydration adds a certain amount of acetone and mixes and stir, and makes that contained oil is dissolved in acetone in the rapeseed oil residue, removes upper strata oil-containing acetone after leaving standstill; Aforesaid method operation 3 times, thoroughly remove institute's oil-containing in the rapeseed oil residue, vacuum-drying subsequently, namely get powder lecithin, gained powder lecithin and 95% ethanol are mixed, put into the thermostatically heating magnetic stirring apparatus, stirring and leaching, separate then, the gained alcohol insoluble solids is first through ether dissolution, the back acetone precipitation, throw out gets thick PE through 60 ℃ of dryings of vacuum after 12 hours, be raw material with thick PE, carry out column chromatography in chromatographic column and separate that silica gel for chromatography dress post was prepended in 120 ℃ of baking ovens activation 60 minutes, be eluent with small amounts of chlorine imitation-carbinol (volume ratio is 2: 1), the flow velocity of control eluent is 3mL/ minute, and gained PE product obtains high-purity PE after the vacuum concentration drying, and its purity is 92.5%.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment does according to technical spirit of the present invention.
Claims (4)
1. a method for preparing the high purity kephalin is characterized in that it comprises the steps:
(1) earlier with the rapeseed oil residue centrifugation, the throw out of gained is dry in vacuum drying oven, carries out vacuum hydro-extraction;
(2) rapeseed oil residue after the dehydration adds a certain amount of acetone and mixes and stir, and makes that contained oil is dissolved in acetone in the rapeseed oil residue, removes upper strata oil-containing acetone after leaving standstill; Institute's oil-containing in the rapeseed oil residue is thoroughly removed in aforesaid method operation 2～3 times, and vacuum-drying subsequently namely gets powder lecithin;
(3) gained powder lecithin and 95% ethanol are mixed, put into the thermostatically heating magnetic stirring apparatus, stirring and leaching is separated then, and the gained alcohol insoluble solids is earlier through ether dissolution, and back acetone precipitation, throw out get thick PE after vacuum-drying;
(4) be raw material with thick PE, carrying out column chromatography in chromatographic column separates, silica gel for chromatography dress post is prepended in 120 ℃ of baking ovens and activates 60 minutes, is eluent with small amounts of chlorine imitation-carbinol (volume ratio is 2: 1), and gained PE product obtains high-purity PE after the vacuum concentration drying.
2. the method for preparing the high purity kephalin as claimed in claim 1 is characterized in that: the temperature control of described vacuum drying oven is at 55～63 ℃.
3. the method for preparing the high purity kephalin as claimed in claim 1, it is characterized in that: the described vacuum drying time is 10～15 hours.
4. the method for preparing the high purity kephalin as claimed in claim 1, it is characterized in that: the flow velocity of described eluent is 3mL/ minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110446654 CN103183705A (en) | 2011-12-27 | 2011-12-27 | Method for preparing high purity cephalin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110446654 CN103183705A (en) | 2011-12-27 | 2011-12-27 | Method for preparing high purity cephalin |
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| CN103183705A true CN103183705A (en) | 2013-07-03 |
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| CN 201110446654 Pending CN103183705A (en) | 2011-12-27 | 2011-12-27 | Method for preparing high purity cephalin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104585761A (en) * | 2015-01-16 | 2015-05-06 | 福建农林大学 | Marine animal phospholipid microcapsule and preparation method thereof |
| CN104592293A (en) * | 2014-12-30 | 2015-05-06 | 广州白云山汉方现代药业有限公司 | Method for preparing high-content phosphatidyl ethanolamine |
| CN112461705A (en) * | 2021-01-21 | 2021-03-09 | 江苏曼氏生物科技股份有限公司 | Method for detecting sterol glycoside content in refined medicinal soybean phospholipid |
| CN114539310A (en) * | 2022-01-28 | 2022-05-27 | 江南大学 | Method for preparing high-purity phosphatidylethanolamine by adsorption method |
| CN115736016A (en) * | 2022-10-20 | 2023-03-07 | 南昌大学 | Preparation method of breast milk phospholipid analogue |
-
2011
- 2011-12-27 CN CN 201110446654 patent/CN103183705A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592293A (en) * | 2014-12-30 | 2015-05-06 | 广州白云山汉方现代药业有限公司 | Method for preparing high-content phosphatidyl ethanolamine |
| CN104592293B (en) * | 2014-12-30 | 2017-03-15 | 广州白云山汉方现代药业有限公司 | A kind of preparation method of high-load PHOSPHATIDYL ETHANOLAMINE |
| CN104585761A (en) * | 2015-01-16 | 2015-05-06 | 福建农林大学 | Marine animal phospholipid microcapsule and preparation method thereof |
| CN112461705A (en) * | 2021-01-21 | 2021-03-09 | 江苏曼氏生物科技股份有限公司 | Method for detecting sterol glycoside content in refined medicinal soybean phospholipid |
| CN114539310A (en) * | 2022-01-28 | 2022-05-27 | 江南大学 | Method for preparing high-purity phosphatidylethanolamine by adsorption method |
| CN115736016A (en) * | 2022-10-20 | 2023-03-07 | 南昌大学 | Preparation method of breast milk phospholipid analogue |
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Application publication date: 20130703 |