CN1072671C - Fine separation of high-purity phospholipid - Google Patents

Abstract

The present invention relates to a fine separation method for high-purity phospholipid. Soybean oil sediments are used as raw materials, and the high-purity phospholipid is prepared by extraction by hexane, impurity removal, decoloring, hexane recovery, extraction by acetone and phospholipids separation. The present invention is characterized in that three-stage systematic fine separation is adopted; firstly, the oil sediments and water are separated from mechanical impurities; secondly, the phospholipid is separated from inorganic impurities; finally, trace impurities in the phospholipid are finely separated by using a high-speed liquid-liquid separation technique, an emulsifying extraction technique and a slightly cooling drying technique. The product has high purity, the purity of fine phospholipid paste is 70%, and the comprehensive indexes of the fine phospholipid paste can reach food-grade indexes; the purity of high-purity phospholipid powder is 98%, and the comprehensive indexes of the high-purity phospholipid powder can reach medicine-grade indexes.

Description

Fine separation of high-purity phospholipid

The present invention relates to a kind of fine separation of high-purity phospholipid.

Phosphatide is natural surface active agent, and distinctive biological activity of tool and physiological function are widely used in foodstuffs industry, medicine industry, cosmetic industry etc.Be mainly used in development trophicity medicament, health giving quality food, heath food, food emulsifier and industrial auxiliary agent.To the prevention heart, cerebrovascular disease, fatty liver, hypertension, hyperlipidemia, obesity, anti-ageing, brain tonic, beauty treatment etc. all is the important biological material.

Confirm that after deliberation phosphatide raw material the most with practical value is soybean and yolk at present.Wherein soybean to contain phosphatide be 1.5～3%, particularly contain 40～50% phosphatide in the oil foot of soyabean processing soya-bean oil, at present mainly by isolating phosphatide in the soybean oil residue.The Separation Research of phosphatide starts from Germany in nineteen twenty, and states such as U.S., Europe and Japan are with raw phospholipid, smart phosphatide separation industriesization since the sixties, and the phosphatide Separation Research has been popular research topic in U.S., Europe, day since the second half eighties.Separating phospholipids from soybean oil residue such as the developed country U.S., Germany, Japan is all used hexane and the extraction of acetone secondary solvent at present, hexane extract is decoloured, adopt common centrifugation impurity such as moisture content wherein, adopt common filter processing mechanical impurity wherein, residual solvent is removed in underpressure distillation.Exist phospholipids content not high with the isolating phosphatide of these class methods, impurity separates unclean, does not reach the high request of food grade, pharmaceutical grade.Phospholipids content is up to 66% in the paste phosphatide of aforesaid method production, and phospholipids content is up to 95% in the powdered phospholipid.As the product that German LucasMeyer company, U.S. CentralSoya company and Soyalecithin company produce, patent JP3128538,890713, EP372327,891124, SU1768169,891212, JP3141288,891024, EP431709, the product that 901206 methods are produced.

The object of the present invention is to provide a kind of fine separation of high-purity phospholipid, make that phospholipids content reaches 70% in the paste phosphatide, the powdered phospholipid phospholipids content reaches 98%, so that high quality food level, pharmaceutical grade phosphatide to be provided.

In order to achieve the above object, method of the present invention realizes by the following method: it is raw material that the present invention adopts preparation of soya-oil dregs, and through hexane extraction, dewater, decolour, reclaim hexane, acetone extract, separating phospholipids and finish, its main points are:

(1) oil foot is come unstuck, vacuum hydro-extraction and filtration, raw phospholipid;

(2) hexane extraction operation, with raw phospholipid and hexane, by 1: 5 volumetric ratio, temperature 30 ℃ ± 2,90～100 rev/mins of revolutions stir extraction 45 minutes, get after the extraction liquid sedimentation removed water in 6 hours, with rotating speed is 10000～12000 rev/mins the meticulous removal of impurities of high velocity liquid liquid separator, then through decolouring, adopts the economic benefits and social benefits thin film distillation to get the smart phosphatide of paste;

(3) the smart phosphatide of paste is repeated (2) operation and get the meticulous phosphatide of paste;

(4) acetone extract operation is pressed 1: 7 volumetric ratio, temperature control 25 ℃ ± 2 with meticulous phosphatide of paste and acetone, stir with 2000～6000 rev/mins rotating speeds, carry out emulsification and extraction 15 minutes, and under 600～640mmHg vacuum tightness, filtered then, get the wet body thing of the meticulous phosphatide of powdery;

(5) the wet body thing of the meticulous phosphatide of powdery is repeated (4) operation and get the wet body thing of the high-purity phosphatide of powdery;

(6) with the wet body thing of the high-purity phosphatide of powdery, shallow cool-drying is to water content below 0.5% under-5 ℃ ± 2 temperature;

(7) with the high-purity phosphatide of dry powdery under nitrogen protection, being crushed to fineness is 120 orders/cm ², get the high-purity phosphatide of powdery.

The present invention has adopted the three-level system fine separation, at first oil foot is separated with mechanical impurity with moisture content; Secondly phosphatide is separated with inorganic impurity; The 3rd introduces high velocity liquid liquid isolation technique, emulsification and extraction technology, economic benefits and social benefits thin film distillation technology, shallow cool-drying technology with the trace impurity in the phosphatide carries out fine separation, so product purity height, the smart phospholipid purity 70% (prior art is 66%) of paste, its comprehensive index reaches food grade; The high-purity phospholipid purity of powdery is 98% (prior art is 96%), and index reaches pharmaceutical grade comprehensively.

Further specify technical scheme of the present invention below in conjunction with embodiment.

(1) soybean oil residue is come unstuck, vacuum hydro-extraction and filtration, raw phospholipid.

(2) the smart phosphatide preparation of paste

1., raw phospholipid and hexane are pressed 1: 5 volumetric ratio, temperature 30 ℃ ± 2,90～100 rev/mins of revolutions; Stir extraction 45 minutes, got the extraction liquid sedimentation 6 hours, make extraction liquid and water stratification, water is removed.

2., extraction liquid is moved in the high rotating speed liquid liquid separator, under 10000～12000 rev/mins of rotating speeds, remove trace impurity and minor amount of water;

3., the extraction liquid after the removal of impurities is placed the redox still, adding its weight 0.8～1% lactic acid accent pH value is 4～5, adds the hydrogen peroxide of extraction liquid weight 7～9% again, temperature control 45 ℃ ± 2, react decolouring in 3.5 hours, being neutralized to acid number with sodium hydroxide then is below 30.

4., the extraction liquid after will decolouring places still kettle, temperature control 60 ℃ ± 2, underpressure distillation under vacuum tightness 600～640mmHg, paste phosphatide;

5., with paste phosphatide from multiple above-mentioned 1., 2., 3., 4. operation gets the meticulous phosphatide of paste.

(3) preparation of the high-purity phosphatide of powdery

1., meticulous phosphatide and acetone are pressed 1: 7 volumetric ratio, temperature control 25 ℃ ± 2, stir with 2000～6000 rev/mins rotating speeds, carried out emulsification and extraction 15 minutes, vacuum filtration under 600～640mmHg vacuum tightness then, with separating organic matters such as smart phosphatide and neutral oil, lipid acid, amino acid, sterol, carbohydrates, the wet body thing of the meticulous phosphatide of powdery.

2., with the meticulous phosphatide of powdery, carry out emulsification and extraction and vacuum filtration once more by last condition 1. and get the wet body thing of the high-purity phosphatide of powdery.

3., with the wet body thing of the high-purity phosphatide of powdery, under-5 ℃ ± 2 temperature, shallow cool-drying is to water content below 0.5%.

4., with the high-purity phosphatide of dry powdery under the protection of nitrogen, being crushed to fineness is 120 orders/cm ², get the high-purity phosphatide of pharmaceutical grade powdery.

The meticulous phosphatide of paste and the high-purity phosphatide technical indicator of powdery of producing with method of the present invention are as follows:

(1) the meticulous phosphatide of paste, liquid state, trade(brand)name paste Yelkin TTS.Soya?Lec-itnin-“Yilkinds”。

(1), state: thickness flows under fluidised form, transparent feel, the normal temperature.

(2), acetone insoluble matter (%): 70

(3), benzene insoluble (%):＜0.3

(4), hexane undissolved substance (%): 0.05

(5), moisture content (%): 1

(6), acid number (mgKOH/g): 20

(7), peroxide value (mg equivalent/kg):＜10

(8), color and luster (Gardner.as.is): 12

(9), mucus (Stoke77 ℃): 65～85

(10), heavy metal (ppm):＜20

(2) high-purity phosphatide

(1), state: Fen Droplets shape, yellowish white

(2), acetone insoluble matter (%): 98

(3), benzene insoluble (%): 0.3

(4), hexane undissolved substance (%): 0.05

(5), moisture content: 0.5

(6), acid number (SZ) (mgKOH/g):＜20

(7), iodine number (IZ): 80～85

(8), peroxide value (POZ):＜10

(9), heavy metal (ppm):＜15

(10), volatile component (In, 105 ℃) %:＜2

Claims (1)

1, a kind of fine separation of high-purity phospholipid, adopting the soybean oil oil foot is raw material, through hexane extraction, dewater, decolouring, hexane recovery, acetone extract, separating phospholipids finish, it is characterized in that:

(1) oil foot is come unstuck, vacuum hydro-extraction and filtration, raw phospholipid;

(2) hexane extraction operation, with raw phospholipid and hexane, by 1: 5 volumetric ratio, temperature 30 ℃ ± 2,90～100 rev/mins of revolutions stir extraction 45 minutes, get after the extraction liquid sedimentation removed water in 6 hours, with rotating speed is 10000～12000 rev/mins the meticulous removal of impurities of high velocity liquid liquid separator, then through decolouring, adopts the economic benefits and social benefits thin film distillation to get the smart phosphatide of paste;

(3) the smart phosphatide of paste is repeated (2) operation and get the meticulous phosphatide of paste;

(4) acetone extract operation is pressed 1: 7 volumetric ratio, temperature control 25 ℃ ± 2 with meticulous phosphatide of paste and acetone, stir with 2000～6000 rev/mins rotating speeds, carry out emulsification and extraction 15 minutes, and under 600～640mmHg vacuum tightness, filtered then, get the wet body thing of the meticulous phosphatide of powdery;

(5) the wet body thing of the meticulous phosphatide of powdery is repeated (4) operation and get the wet body thing of the high-purity phosphatide of powdery;

(6) with the wet body thing of the high-purity phosphatide of powdery, shallow cool-drying is to water content below 0.5% under-5 ℃ ± 2 temperature;

(7) with the high-purity phosphatide of dry powdery under nitrogen protection, being crushed to fineness is 120 orders/cm ², get the high-purity phosphatide of powdery.