CN1974582A - Supersonically reinforced yolk phospholipid extracting process - Google Patents

Supersonically reinforced yolk phospholipid extracting process Download PDF

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Publication number
CN1974582A
CN1974582A CN 200610123974 CN200610123974A CN1974582A CN 1974582 A CN1974582 A CN 1974582A CN 200610123974 CN200610123974 CN 200610123974 CN 200610123974 A CN200610123974 A CN 200610123974A CN 1974582 A CN1974582 A CN 1974582A
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CN
China
Prior art keywords
extraction
yolk powder
gallus domesticus
ovum gallus
domesticus flavus
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CN 200610123974
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Chinese (zh)
Inventor
周锦珂
李金华
葛发欢
杨祖金
曾荣华
邹小燕
陈德建
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Hanfang Modem Chinese Traditional Medicine Research Development Co Ltd Guang
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Hanfang Modem Chinese Traditional Medicine Research Development Co Ltd Guang
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Priority to CN 200610123974 priority Critical patent/CN1974582A/en
Publication of CN1974582A publication Critical patent/CN1974582A/en
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Abstract

The supersonically reinforced process of extracting yolk phospholipid with yolk powder containing protein and fat as material includes supersonically reinforced extraction of yolk powder in 80-99 % concentration alcohol solution of 3-20 times weight of yolk powder at 20-70 deg.c for 1-3 times 0.1-1 hr each, with the supersonic wave frequency being 20-150 KHz; centrifuging and filtering the extracted liquid; and decompression concentrating the supernatant and vacuum drying to obtain yolk phospholipid. Compared with available processes, the present invention has the advantages of simple operation, short extraction period, low power consumption, low extraction cost, high effective component transferring rate, etc.

Description

The method of supersonically reinforced yolk phospholipid extracting
Technical field
The present invention relates to a kind of is raw material to contain albumen with fatty yolk powder, extracts the method for effective active composition, specifically relates to a kind of method of utilizing ultrasound-enhanced extractive technique to extract Ovum Gallus domesticus Flavus lecithin from yolk powder.
Background technology
Yelkin TTS is that a class mainly is made up of phosphatidylcholine (PC), phosphatidylethanolamine (PE), sphingomyelin (SM), lipositol, silk phosphatide and phosphatidic acid etc., and have the important substance of obvious physiologically active, be widely used in fields such as medicine, food, chemical industry, light industry at present.Yelkin TTS is except that a small amount of synthetic, and main source is to extract to obtain from natural phant or animal powdered egg, as soybean phospholipid that extracts from soybean or the egg phospholipids that extraction obtains from yolk.
External and the clinical study of having carried out both at home and abroad proves, Yelkin TTS energy dissolving cholesterol and triglyceride level, keep unobstructed blood vessel, effective preventing hypertension, hyperlipidemia and multiple cardiovascular and cerebrovascular disease, can directly enter by hemato encephalic barrier again and participate in the synthetic of neurotransmitter acetylcholine in the brain, play brain.Simultaneously, because existing hydrophilic radical in the lecithin molecules has oil loving group again, be the naturally occurring emulsifying agent of stable performance, safety, because its applied range, the Ovum Gallus domesticus Flavus lecithin demand is growing.Therefore, research and development Ovum Gallus domesticus Flavus lecithin preparation technology and realize that its industrialization is a crucial research topic, has remarkable economical meaning and social effect.
Ovum Gallus domesticus Flavus lecithin mainly contains solvent-extraction process and supercritical CO at present on extraction process 2Extraction process.The extraction solvent that traditional solvent relates generally to has alkanes, acetone, dme, C 1~C 3The binary system of Fatty Alcohol(C12-C14 and C12-C18) or Fatty Alcohol(C12-C14 and C12-C18) and alkane, ubiquitous problem are that the organic solvent consumption is big, the process time is long, extract yield Yelkin TTS is on the low side etc., are unfavorable for the suitability for industrialized production of product." Gansu Agriculture University,'s journal " 2003 the 38th the 3rd phases of volume " optimum process condition of extraction Yelkin TTS in the egg yolk " disclose and have adopted organic solvent to extract the operational path of Yelkin TTS from yolk, use earlier the analytical pure acetone deoiling, resulting throw out is used 99.7% extraction using alcohol again, and extracting solution is concentrated, is drying to obtain product.This technology is not only had relatively high expectations to solvent, and last resulting phosphatide yield is on the low side only to be 19.216%.
Supercritical carbon dioxide extraction method can be from yolk powder the higher Ovum Gallus domesticus Flavus lecithin of dna purity.The CN1056375C patent disclosure a kind of method of from yolk powder, extracting Ovum Gallus domesticus Flavus lecithin with supercritical co, this method can be isolated Oil of egg yolk and Ovum Gallus domesticus Flavus lecithin, but extraction time length is 3~4hr, working pressure is at 16~26MPa, there are problems such as facility investment is big, maintenance cost is high, production cost is higher, make commercial application be subjected to certain restriction.
In order to overcome the shortcoming of above-mentioned two kinds of extracting method, be necessary to grope a kind of new method for preparing Ovum Gallus domesticus Flavus lecithin.
Summary of the invention
The objective of the invention is from yolk powder, to extract Ovum Gallus domesticus Flavus lecithin, improve Yelkin TTS extraction yield in the yolk powder, simplify production technique, reduce production costs.
In order to reach the used technical scheme of goal of the invention be: with yolk powder is that raw material adopts the method for ultrasound-enhanced extraction to extract Ovum Gallus domesticus Flavus lecithin from yolk powder, be about to yolk powder and place the supersound extraction container, the ethanolic soln of adding 80~99%, ultrasound-enhanced extraction is 1~3 time under the whipped state, add ethanolic soln cumulative volume be 3~20 times of yolk powder weight, its ultrasonic frequency is 20~150KHz, extracting temperature is 20~70 ℃, each extraction time is 0.1~1hr, material after the supersound extraction is through centrifugal or filtration, clear liquid obtains Ovum Gallus domesticus Flavus lecithin through concentrating under reduced pressure and drying.
During concrete operations can be get clear liquid 40 ℃~45 ℃ of temperature, vacuum tightness-0.085MPa~-be evaporated to thick paste under the 0.095MPa condition, reclaim solvent, resulting paste in 55 ℃~60 ℃ of temperature, vacuum tightness-0.085MPa~-the 0.095MPa condition under drying under reduced pressure, promptly get light yellow Ovum Gallus domesticus Flavus lecithin.
Through the preferred processing condition of experimental study repeatedly be add ethanolic soln volume be preferably 6~15 times of yolk powder weight; Ultrasonic frequency during supersound extraction is 20~70KHz, and extracting temperature is 25~45 ℃, and each extraction time is 15min~40min; The pattern that supersound extraction adopted is that probe type ultrasonic or cleaning type are ultrasonic.
Patent of the present invention has overcome the deficiency of traditional solvent and supercritical carbon dioxide extraction Ovum Gallus domesticus Flavus lecithin technology.Because supersound extraction is to utilize multiple-effects such as ultrasonic cavitation effect, mechanical shock, heat effect, the High Temperature High Pressure field that moment produces in fluid, solid surface in the convection cell produces powerful shearing force, quicken the stripping and the reinforcing mass transfer process of active skull cap components, promote the mass transfer that extracts composition to separate, thereby shorten extraction time, improve extraction efficiency.This patent adopts ultrasound-enhanced extractive technique to extract Yelkin TTS from yolk powder and compares with existing method, have easy and simple to handle, extraction time is short, production energy consumption is low, extraction cost is low, the rate of transform height of effective constituent, production process safely, be easy to the advantage of aspects such as suitability for industrialized production.
Ultrasound-enhanced extractive technique is to strengthen under the leaching process at low-temperature physics to carry out resulting product purity height, good stability.Biological activity keeps intact, has kept the natural radioactivity and the trophic function characteristic of Ovum Gallus domesticus Flavus lecithin to greatest extent, meets the requirement of present people to the natural nutrition health functional food.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further elaborated, the scheme of embodiment described here does not limit the present invention.
The described rate of recovery of following examples, assay, yolk powder raw material and ultrasonic device are described as follows:
2006 the 24th the 4th phases of volume of lecithin content measuring method reference literature " chromatogram " " high performance liquid chromatography-evaporative light scattering detection method is measured the content of Ovum Gallus domesticus Flavus lecithin ".
The pasteurize yolk powder that the yolk powder raw material adopts Shaanxi Tiandou Egg Droduct Industry Co., Ltd. to produce, lecithin content is 14.2%.
Ultrasonic device is available from Jining gold hundred special Electronics Co., Ltd.s, and model specification is GDC-TQ/ZS/3.
Embodiment 1
Take by weighing the 1kg yolk powder, place cleaning type supersound extraction container, add 80% ethanolic soln 3L, it is 20KHz that ultrasonic frequency is set, ultrasonic time 0.1hr, 20 ℃ of supersound extraction temperature.In supersound extraction once, the feed liquid of supersound extraction is collected clear liquid after filtration under whipped state.With clear liquid 40 ℃~45 ℃ of temperature, vacuum tightness-0.085MPa~-be evaporated to thick paste under the 0.095MPa condition, reclaim solvent, with resulting paste in 45 ℃~50 ℃ of temperature, vacuum tightness-0.085MPa~-the 0.095MPa condition under drying under reduced pressure, obtain light yellow Ovum Gallus domesticus Flavus lecithin 154g, measuring lecithin content with HPLC is 60.9%, and the rate of recovery is 65.9%.
Embodiment 2
Ultrasonic device, raw material and operating process used among the embodiment 2 are with embodiment 1, and different is that ultrasonic extraction solvent is 85% ethanolic soln 6L, and the supersound extraction temperature is 25 ℃, supersound extraction time 1hr.The light yellow Ovum Gallus domesticus Flavus lecithin 179g for preparing under these processing condition, lecithin content is 64.1%, the rate of recovery is 80.7%.
Embodiment 3
Ultrasonic device, raw material and operating process used in the present embodiment are with embodiment 1, different is to do following adjustment in relevant ultrasound-enhanced extraction process parameter: added solvent is 90% ethanolic soln 15L, ultrasonic frequency 45KHz, the supersound extraction temperature is 45 ℃, extraction time 0.3hr.The prepared Ovum Gallus domesticus Flavus lecithin finished weight of this law is 190g, and lecithin content is 71.2%, and the rate of recovery is 95.3%.
Embodiment 4
Take by weighing with embodiment 1 with lot number yolk powder raw material 1kg, place cleaning type supersound extraction container, add 12 liter of 95% ethanolic soln in the extraction vessel, it is 26KHz that ultrasonic frequency is set, ultrasonic time 0.5hr, the supersound extraction temperature is 25 ℃, under whipped state in supersound extraction once.Material is extracted in centrifugation, obtains clarifying extracting solution.The concentrating of extracting solution, dry subsequent processes are same with embodiment 1.This legal system gets Ovum Gallus domesticus Flavus lecithin weight 187g, and lecithin content is 73.8%, and the rate of recovery is 97.4%.
Embodiment 5
Present embodiment institute adopting process parameter is all identical with embodiment 4, and different is supersound extraction equipment, and the supersound extraction pattern that present embodiment adopts is that probe type ultrasonic extracts.This legal system gets Ovum Gallus domesticus Flavus lecithin weight 188g, and lecithin content is 73.1%, and the rate of recovery is 96.8%.
Embodiment 6
Ultrasonic device, raw material and operating process used among the embodiment 6 are with embodiment 1, and the part processing parameter is adjusted as follows, and used extraction solvent is 95% ethanol 15L, and ultrasonic frequency is 70KHz, and the supersound extraction temperature is 35 ℃, ultrasonic time 0.7hr.The light yellow Ovum Gallus domesticus Flavus lecithin 189g for preparing under these processing condition, lecithin content is 72.5%, the rate of recovery is 96.4%.
Embodiment 7
Ultrasonic device, raw material and operating process used among the embodiment 7 are with embodiment 1, and different is that the used solvent of supersound extraction is 95% ethanolic soln 12L, and ultrasonic frequency is set to 100KHz, and the supersound extraction temperature is 60 ℃, and extraction time is 1hr.According to the resulting Ovum Gallus domesticus Flavus lecithin weight of this law 191g, lecithin content is 68.8%, and the rate of recovery is 92.4%.
Embodiment 8
Take by weighing with embodiment 1 with lot number yolk powder raw material 1kg, place cleaning type supersound extraction container, set following ultrasound parameter: ultrasonic frequency is 150KHz, the supersound extraction temperature is 70 ℃, extracting solvent is 99% ethanolic soln, extract three times, the each extraction adds solvent 6L, and each extraction time is 0.6hr.The concentrating of extracting solution, dry subsequent processes are same with embodiment 1.The Ovum Gallus domesticus Flavus lecithin weight 211g for preparing under these processing condition, lecithin content is 61.2%, the rate of recovery is 90.8%.
Embodiment 9
Adopt traditional alcohol extraction process of bibliographical information, get the 1kg yolk powder and place extraction vessel, add 95% ethanolic soln 12L, 25 ℃ of extractions of temperature once, extraction time is 0.5hr.The filtration of extracting solution, concentrate, dry subsequent processes is same with embodiment 1.Adopt the Ovum Gallus domesticus Flavus lecithin weight 168g of traditional alcohol extraction process condition preparation of bibliographical information, lecithin content is 62.3%, and the rate of recovery is 73.7%.
Embodiment 10
Adopt traditional alcohol extraction process of bibliographical information, get the 1kg yolk powder and place extraction vessel, add 80% ethanolic soln 3L, 20 ℃ of extractions of temperature once, extraction time is 0.1hr.The filtration of extracting solution, concentrate, dry subsequent processes is same with embodiment 1.Adopt the Ovum Gallus domesticus Flavus lecithin weight 55g of traditional alcohol extraction process condition preparation of bibliographical information, lecithin content is 58.3%, and the rate of recovery is 22.6%.
The experimental result of the foregoing description gathers following table
Adopt ultrasound-enhanced extraction as can be seen by summary sheet as a result, the method optimum of embodiment 4, the method rate of recovery of embodiment 10 is minimum.Embodiment 9 does not add ultrasound-enhancedly, and other extraction conditions and embodiment 4 are identical, and the Ovum Gallus domesticus Flavus lecithin rate of recovery is respectively 73.7% and 97.4% but extract as a result, and embodiment 4 has improved 23.7% than embodiment 9, has significant difference.Embodiment 10 does not add ultrasound-enhancedly, and other extraction conditions and embodiment 1 are identical, and the Ovum Gallus domesticus Flavus lecithin rate of recovery is respectively 22.6% and 65.9% but extract as a result, and embodiment 1 has improved 43.3% than embodiment 10, has significant difference.
Because supersound extraction is to utilize multiple-effects such as ultrasonic cavitation effect, mechanical shock, heat effect, the High Temperature High Pressure field that moment produces in fluid, solid surface in the convection cell produces powerful shearing force, quicken the stripping and the reinforcing mass transfer process of active skull cap components, promote the mass transfer that extracts composition to separate.Therefore, adopt ultrasound-enhanced extraction method from yolk powder, to extract the traditional extraction process reduced in comparison extraction time of Yelkin TTS and bibliographical information, improve extraction efficiency.

Claims (3)

1, a kind of extracting method of Ovum Gallus domesticus Flavus lecithin, be to be raw material with the yolk powder, with the ethanolic soln is that solvent extracts, it is characterized in that yolk powder is placed the supersound extraction container, the ethanolic soln of adding 80~99%, ultrasound-enhanced extraction is 1~3 time under the whipped state, add ethanolic soln cumulative volume be 3~20 times of yolk powder weight, its ultrasonic frequency is 20~150KHz, extracting temperature is 20~70 ℃, and each extraction time is 0.1~1hr, and the material after the supersound extraction is through centrifugal or filtration, clear liquid concentrating under reduced pressure and drying obtain Ovum Gallus domesticus Flavus lecithin.
2, the extracting method of Ovum Gallus domesticus Flavus lecithin according to claim 1, the cumulative volume that it is characterized in that described interpolation ethanolic soln are 6~15 times of yolk powder weight.
3, the extracting method of Ovum Gallus domesticus Flavus lecithin according to claim 1, the ultrasonic frequency when it is characterized in that described ultrasound-enhanced extract is 20~70KHz, extracts 25~45 ℃ of temperature, each extraction time is 15min~40min.
CN 200610123974 2006-12-01 2006-12-01 Supersonically reinforced yolk phospholipid extracting process Pending CN1974582A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102863470A (en) * 2012-09-10 2013-01-09 江苏大学 Method for coproducing egg yolk lecithin, cephalin, yolk oil and low-denatured protein flour
CN102863469A (en) * 2012-09-10 2013-01-09 江苏大学 Preparation method of high-purity egg yolk phosphatidylcholine (PC)
CN106728370A (en) * 2016-12-15 2017-05-31 毛美香 The preparation method for promoting the Chinese medicine of black hair
CN108181143A (en) * 2017-12-12 2018-06-19 山东金胜粮油集团有限公司 A kind of method of quick detection grease phosphorus content

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102863470A (en) * 2012-09-10 2013-01-09 江苏大学 Method for coproducing egg yolk lecithin, cephalin, yolk oil and low-denatured protein flour
CN102863469A (en) * 2012-09-10 2013-01-09 江苏大学 Preparation method of high-purity egg yolk phosphatidylcholine (PC)
CN102863469B (en) * 2012-09-10 2015-04-22 江苏大学 Preparation method of high-purity egg yolk phosphatidylcholine (PC)
CN106728370A (en) * 2016-12-15 2017-05-31 毛美香 The preparation method for promoting the Chinese medicine of black hair
CN108181143A (en) * 2017-12-12 2018-06-19 山东金胜粮油集团有限公司 A kind of method of quick detection grease phosphorus content

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