CN103013653B - Preparation method of refined egg oil - Google Patents
Preparation method of refined egg oil Download PDFInfo
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- CN103013653B CN103013653B CN201210580024.XA CN201210580024A CN103013653B CN 103013653 B CN103013653 B CN 103013653B CN 201210580024 A CN201210580024 A CN 201210580024A CN 103013653 B CN103013653 B CN 103013653B
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Abstract
The invention discloses a preparation method of refined egg oil. The preparation method comprises the steps of: supercritically extracting yolks to obtain crude egg oil; dissolving by using an organic solvent as a solvent (adding 1L of organic solvent to 1kg of crude egg oil to dissolve) and stirring; standing and precipitating, taking supernate to flow into an alumina column, adding the rest of precipitate into the alumina column, continuously eluting by using the organic solvent (eluting 1kg of alumina by using 2-6L of organic solvent), combining eluents, and concentrating to obtain egg oil; continuously adding hargil, reducing pressure and stirring at 100-150 DEG C, cooling and filtering to remove hargil to obtain the refined egg oil with low cholesterol, acid value and peroxide value. The preparation method has the characteristics of convenience for operation, low energy consumption and the like and meets the demands of industrial batch production.
Description
technical field:
The present invention relates to the refining purification technique of Oil of egg yolk, specifically, relate to the refine yolk oil preparation method of a kind of low-cholesterol, low acid number, low peroxide value.
background technology:
In Oil of egg yolk, main component has triglyceride level, a small amount of free fatty acids, pigment etc.Yolk triglyceride level is the important nutritive substances of the mankind, when body metabolism is oxidized, can produce a large amount of heats.Because the lipid acid composition of Oil of egg yolk is similar to human milk, be therefore used as the base oil in infant formula.It also can be used as the auxiliary material of the full Liposyn of the high nutrition of urgent patient, and patient health is played an important role with sustaining life.In addition, Oil of egg yolk also has the effects such as anti-inflammatory, treatment scald.In the Oil of egg yolk that tradition is extracted, cholesterol level is higher, affects the extensive application of Oil of egg yolk, and the higher Oil of egg yolk that also easily makes of acid number and peroxide value is rotten simultaneously.Therefore, prepare lower cholesterol content, low acid number, the high-quality refine yolk oil of low peroxide value will be conducive to applying of Oil of egg yolk, be conducive to improve the comprehensive utilization ability to this agricultural byproducts resource of yolk, be conducive to take a firm foundation for preparing medicinal refine yolk oil.
In < < Chinese Pharmacopoeia > > 2010 editions, lack the record of the relevant purification refine of Oil of egg yolk, and in document to Oil of egg yolk mainly extract purification refine technique be mainly SCF-CO 2, solvent extraction and-cyclodextrin inclusion technique.
Chinese patent < < provides and utilizes postcritical extracting method with the method > > of CO2 supercritical extraction Root of Convolvulate Asiabell butter and the method > > of < < supercritical CO 2 continuous extraction Oil of egg yolk and Ovum Gallus domesticus Flavus lecithin, but the follow-up purification refine that do not continue, residual a large amount of cholesterol, affects quality and the range of application of Oil of egg yolk.
The method for making of Chinese patent < < obtaining high-purity egg oil and application > > thereof utilize solvent extraction to refine Oil of egg yolk, but extraction times is many, solvent load is greatly its shortcoming, and extraction process is difficult to cholesterol to be removed completely.
< < China livestock products and food > > have reported that a kind of alcohol percolation method that utilizes extracts Oil of egg yolk from yolk powder in the 7th 5 phases of volume " extraction of Oil of egg yolk and composition analysis " in 2000, but its cholesterol level reaches 5.4%, directly application affects HUMAN HEALTH.
Chinese patent < < natural yolk oil extracting process > > utilizes high temperature from yolk, to extract Oil of egg yolk, but because temperature is higher, time is grown and is difficult to carry out under vacuum state, easily cause that in Oil of egg yolk, the structure of matter changes, thereby cause the quality index such as acid number, peroxide value defective.
The method > > that mono-kind of Chinese patent < < extracts Yelkin TTS, Oil of egg yolk and cholesterol from yolk provides a kind of and from yolk fluid, extracts Yelkin TTS with ethanol,-cyclodextrin is except de-cholesterol, thereby refine out the method for Oil of egg yolk, this method is due to residual Yelkin TTS and cholesterol, and Oil of egg yolk is of low quality.
, all there is the residual height of cholesterol in the extraction and purification process document of comprehensive existing Oil of egg yolk, acid number, and peroxide values etc. affect the problem of stability indicator.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of low-cholesterol is provided, the preparation method of acid number, refine yolk oil that peroxide value is qualified.
In order to realize above-mentioned object, the present invention takes following scheme: a kind of preparation method of refine yolk oil, comprise the steps: yolk powder to obtain thick Oil of egg yolk through supercritical extraction, with organic solvent, as dissolution with solvents, stir (the thick Oil of egg yolk of every 1kg adds 1L organic solvent dissolution); Staticly settle, get supernatant liquor and pass through alumina column, and remaining throw out is added in alumina column in the lump, with organic solvent, continue wash-out (the organic solvent wash-out of 2 ~ 6L for every 1kg aluminum oxide) again, the Oil of egg yolk obtaining after elutriant merging is concentrated continues to add carclazyte, at 100 ~ 150 ℃, decompression is stirred, and lets cool rear suction filtration and removes carclazyte and obtain refine yolk oil.
In the preparation method of above-mentioned refine yolk oil, described alumina column aluminum oxide used is neutral alumina, acidic alumina or alkali alumina.
In the preparation method of above-mentioned refine yolk oil, in described alumina column, alumina weight is 80% ~ 500% of thick Oil of egg yolk weight.
In the preparation method of above-mentioned refine yolk oil, the footpath post of described alumina column is than being 1:3 ~ 8.
In the preparation method of above-mentioned refine yolk oil, described organic solvent is normal hexane, hexanaphthene.
In the preparation method of above-mentioned refine yolk oil, described carclazyte consumption was 0.5 ~ 5% of the concentrated rear Oil of egg yolk weight of post.
In the preparation method of above-mentioned refine yolk oil, the described decompression stirring operation time is 20 ~ 60min.
In the preparation method of above-mentioned refine yolk oil, described decompression whipping temp is 100 ~ 150 ℃.
In the preparation method of above-mentioned refine yolk oil, 3L organic solvent wash-out for every 1kg aluminum oxide, at 120 ℃, 30min is stirred in decompression.
Compared with prior art, the present invention has following useful effect:
1. the present invention first takes organic solvent to improve the mobility of Oil of egg yolk, and in the technological operation of follow-up reduction peroxide value, more thoroughly removes desolventizing.Due to weather temperature variation, through the thick Oil of egg yolk of supercritical extraction, easily separate out and mobility variation, affect subsequent purification refinement treatment, add organic solvent can effectively make thick Oil of egg yolk mobility improve, improve purification efficiency.After concentration and recovery, most of solvent is removed simultaneously; Follow-up heating under vacuum stirring more again, is conducive to residual solvent and removes.
2. the present invention succinctly removes the free cholesterol in Oil of egg yolk up hill and dale, improves the proterties of Oil of egg yolk.Through the present invention, carry out refining Oil of egg yolk proterties clarification, smell is good, and moisture is removed substantially, not containing free cholesterol.Be conducive to be applied to makeup, the production application of food and medicine.
3. the present invention reduces acid number and the peroxide value in Oil of egg yolk, improves the stability of Oil of egg yolk.Because moisture, acid number and peroxide value are effectively improved, remove the factors of instability in Oil of egg yolk, be conducive to the stably stored of Oil of egg yolk.
embodiment:
Comparative example 1
With reference in the method for making of Chinese patent < < obtaining high-purity egg oil and application > > thereof by the method for organic solvent extraction, utilize dehydrated alcohol extraction 10 times, still there is obvious cholesterol spot in tlc analysis Oil of egg yolk, illustrates that extracting process is difficult to effectively remove cholesterol.
Comparative example 2
Extract from yolk with reference to mono-kind of Chinese patent < < in the method > > of Yelkin TTS, Oil of egg yolk and cholesterol-cyclodextrin inclusion technique is processed Oil of egg yolk, find that tlc analysis Oil of egg yolk still exists obvious cholesterol spot, illustrate-cyclodextrin inclusion technique is difficult to effectively remove cholesterol equally.
Embodiment 1
Yolk powder is obtained to thick Oil of egg yolk through supercritical extraction, with normal hexane, as dissolution with solvents, stir, slightly the weightmeasurement ratio of cholesterol and normal hexane is that 1:1(is that the thick Oil of egg yolk of every 1kg adds 1L n-hexane dissolution).Staticly settle, (aluminum oxide consumption is 1:1 with thick Oil of egg yolk weight ratio by alumina column to get supernatant liquor, footpath post is than being 1:4), and remaining throw out is added in alumina column in the lump, with normal hexane, continue wash-out again, the envelope-bulk to weight ratio of normal hexane and aluminum oxide is that 3:1(is 3L normal hexane wash-out for every 1kg aluminum oxide), elutriant merges the Oil of egg yolk obtaining after concentrated and continues to add 1% carclazyte (being that every 1kg Oil of egg yolk adds 0.01kg carclazyte), at 120 ℃, 30min is stirred in decompression, lets cool rear suction filtration and removes carclazyte and obtain qualified refine yolk oil.Found that, refine yolk oil yield 90%, tlc analysis finds there is no the corresponding spot of cholesterol standard substance in refine yolk oil.Acid number is 0.1, peroxide value 0.6.
Embodiment 2
Yolk powder is obtained to thick Oil of egg yolk through supercritical extraction, with normal hexane, as dissolution with solvents, stir, slightly the weightmeasurement ratio of cholesterol and normal hexane is that 1:1(is that the thick Oil of egg yolk of every 1kg adds 1L n-hexane dissolution).Staticly settle, (aluminum oxide consumption is 5:1 with thick Oil of egg yolk weight ratio by alumina column to get supernatant liquor, footpath post is than being 1:3), and remaining throw out is added in alumina column in the lump, with normal hexane, continue wash-out again, the envelope-bulk to weight ratio of normal hexane and aluminum oxide is that 6:1(is 6L normal hexane wash-out for every 1kg aluminum oxide), the Oil of egg yolk obtaining after elutriant merging is concentrated continues to add 0.5% carclazyte (being that every 1kg Oil of egg yolk adds 0.005kg carclazyte), at 100 ℃, 60min is stirred in decompression, lets cool rear suction filtration and removes carclazyte and obtain qualified refine yolk oil.Found that, refine yolk oil yield 86%, tlc analysis finds there is no the corresponding spot of cholesterol standard substance in refine yolk oil.Acid number is 0.1, peroxide value 0.9.
Embodiment 3
Yolk powder is obtained to thick Oil of egg yolk through supercritical extraction, is that dissolution with solvents stirs with cyclohexane give, and the weightmeasurement ratio of thick cholesterol and hexanaphthene is that 1:1(is that the thick Oil of egg yolk of every 1kg adds the dissolving of 1L hexanaphthene).Staticly settle, (aluminum oxide consumption is 5:6 with thick Oil of egg yolk weight ratio by alumina column to get supernatant liquor, footpath post is than being 1:8), and remaining throw out is added in alumina column in the lump, with hexanaphthene, continue wash-out again, the envelope-bulk to weight ratio of hexanaphthene and aluminum oxide is that 2:1(is 2L hexanaphthene wash-out for every 1kg aluminum oxide), the Oil of egg yolk obtaining after elutriant merging is concentrated continues to add 5% carclazyte (being that every 1kg Oil of egg yolk adds 0.05kg carclazyte), at 150 ℃, 20min is stirred in decompression, lets cool rear suction filtration and removes carclazyte and obtain qualified refine yolk oil.Found that, refine yolk oil yield 92%, tlc analysis finds there is no the corresponding spot of cholesterol standard substance in refine yolk oil.Acid number is 0.3, peroxide value 0.4.
Embodiment 4
Yolk powder is obtained to thick Oil of egg yolk through supercritical extraction, with normal hexane, as dissolution with solvents, stir, slightly the weightmeasurement ratio of cholesterol and normal hexane is that 1:1(is that the thick Oil of egg yolk of every 1kg adds 1L n-hexane dissolution).Staticly settle, (aluminum oxide consumption is 5:3 with thick Oil of egg yolk weight ratio by acidic alumina column to get supernatant liquor, footpath post is than being 1:6), and remaining throw out is added in alumina column in the lump, with normal hexane, continue wash-out again, the envelope-bulk to weight ratio of normal hexane and aluminum oxide is that 2:1(is 2L normal hexane wash-out for every 1kg aluminum oxide), the Oil of egg yolk obtaining after elutriant merging is concentrated continues to add 3% carclazyte (being that every 1kg Oil of egg yolk adds 0.03kg carclazyte), at 130 ℃, 40min is stirred in decompression, lets cool rear suction filtration and removes carclazyte and obtain qualified refine yolk oil.Found that, refine yolk oil yield 90%, tlc analysis finds there is no the corresponding spot of cholesterol standard substance in refine yolk oil.Acid number is 0.2, peroxide value 0.6.
Claims (7)
1. the preparation method of a refine yolk oil, it is characterized in that comprising the steps: yolk powder is obtained to thick Oil of egg yolk through supercritical extraction, with organic solvent, as dissolution with solvents, stir and add 1L organic solvent dissolution by the thick Oil of egg yolk of every 1kg, staticly settle, get supernatant liquor and pass through alumina column, and remaining throw out is added in alumina column in the lump, with organic solvent, continue wash-out again, organic solvent wash-out by every 1kg aluminum oxide with 2 ~ 6L, the Oil of egg yolk obtaining after elutriant merging is concentrated continues to add carclazyte, at 100 ~ 150 ℃, decompression is stirred, letting cool rear suction filtration removes carclazyte and obtains refine yolk oil, described organic solvent is normal hexane, hexanaphthene.
2. the preparation method of refine yolk oil according to claim 1, is characterized in that, described alumina column aluminum oxide used is neutral alumina, acidic alumina or alkali alumina.
3. the preparation method of refine yolk oil according to claim 2, is characterized in that, in described alumina column, alumina weight is 80% ~ 500% of thick Oil of egg yolk weight.
4. the preparation method of refine yolk oil according to claim 1, is characterized in that, the footpath post of described alumina column is than being 1:3 ~ 8.
5. the preparation method of refine yolk oil according to claim 1, is characterized in that, described carclazyte consumption was 0.5 ~ 5% of the concentrated rear Oil of egg yolk weight of post.
6. the preparation method of refine yolk oil according to claim 1, is characterized in that, the described decompression stirring operation time is 20 ~ 60min.
7. the preparation method of refine yolk oil according to claim 1, is characterized in that, 3L organic solvent wash-out for every 1kg aluminum oxide, and at 120 ℃, 30min is stirred in decompression.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104177466A (en) * | 2013-05-22 | 2014-12-03 | 广州白云山汉方现代药业有限公司 | Preparation technology for extracting cholesterol from egg yolk oil |
| CN103540402A (en) * | 2013-10-31 | 2014-01-29 | 西南大学 | Method for reducing content of cholesterol in chrysalis oil |
| CN105132152B (en) * | 2015-08-10 | 2018-11-09 | 山西中医学院 | A kind of yolk for acid value analysis evaporates the process for purification of oil |
| CN108084243A (en) * | 2017-12-28 | 2018-05-29 | 广州白云山汉方现代药业有限公司 | A kind of method that high-purity cholesterol is extracted from egg oil |
| CN109456828A (en) * | 2018-12-13 | 2019-03-12 | 中铭生物科技(深圳)有限公司 | A kind of manufacturing method of natural astaxanthin egg oil |
| CN111234920A (en) * | 2019-12-09 | 2020-06-05 | 南京威尔药业股份有限公司 | Refining method of castor oil with low acid value and low chroma |
Citations (2)
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| CN1123557A (en) * | 1994-02-21 | 1996-05-29 | 沃纳·C·诺罗基 | Process for obtaining high-purity egg oil and use thereof |
| CN1476783A (en) * | 2003-07-04 | 2004-02-25 | 迟玉杰 | Method for continuously extracting egg yolk oil and egg yolk lecithin by using supercritical CO2 extraction process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002034513A (en) * | 2000-07-18 | 2002-02-05 | Tsukasa Sakuraba | Method for washing with water, separating and collecting of ultrahigh-purity egg oil corresponding to three kinds of egg yolks |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1123557A (en) * | 1994-02-21 | 1996-05-29 | 沃纳·C·诺罗基 | Process for obtaining high-purity egg oil and use thereof |
| CN1476783A (en) * | 2003-07-04 | 2004-02-25 | 迟玉杰 | Method for continuously extracting egg yolk oil and egg yolk lecithin by using supercritical CO2 extraction process |
Non-Patent Citations (4)
| Title |
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| Removal of sterols from lipid matrix by extraction with compressed lower hydrocarbons, useful e.g. for removing cholesterol from fats or oils or for recovering biologically active sterol derivatives. DE10037515A;无;《德温特数据库》;20021231(第DW200220期);EXAMPLE和摘要附图 * |
| 无.Removal of sterols from lipid matrix by extraction with compressed lower hydrocarbons, useful e.g. for removing cholesterol from fats or oils or for recovering biologically active sterol derivatives. DE10037515A.《德温特数据库》.2002,(第DW200220期),EXAMPLE和摘要附图. |
| 王卫芬.蛋黄油脱酸及蛋黄卵磷脂纯化工艺研究.《中国优秀硕士学位论文全文数据库》.2009,(第3期),第12页2.3.1，第27页2.5（2），第41页3.5（2）以及第38页3.4.8. |
| 蛋黄油脱酸及蛋黄卵磷脂纯化工艺研究;王卫芬;《中国优秀硕士学位论文全文数据库》;20090331(第3期);第12页2.3.1，第27页2.5（2），第41页3.5（2）以及第38页3.4.8 * |
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