CN105132152B - A kind of yolk for acid value analysis evaporates the process for purification of oil - Google Patents
A kind of yolk for acid value analysis evaporates the process for purification of oil Download PDFInfo
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- CN105132152B CN105132152B CN201510482721.5A CN201510482721A CN105132152B CN 105132152 B CN105132152 B CN 105132152B CN 201510482721 A CN201510482721 A CN 201510482721A CN 105132152 B CN105132152 B CN 105132152B
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Abstract
The invention belongs to yolk to evaporate oily preparing technical field, be difficult to carry out acid value analysis deeply to solve the problems, such as that current yolk evaporates strong carcinogen BaP content height, color with oil color in oil, provide a kind of process for purification for being used for the yolk that acid value is analyzed and evaporating oil.It takes yolk obtained by high-temperature retorting to evaporate oil, is placed it in again in supercritical carbon dioxide extraction element after adsorbent stirring and adsorbing is added, adjust extracting parameter, obtain refined yolk and evaporate oil product.It is yellow to light yellow that the refined yolk obtained, which evaporates oily color, and unsaturated fatty acid content is 65.0~75.0%；Harmane alkaloids content rises to 0.035~0.053%, and harmful components Benzpyrene content may decrease to 0.010~0.019%.Harmful substance BaP removal rate is high, and color with oil color is shallow, can be used for acid value analysis, is conducive to stabilised quality, easy to spread.
Description
Technical field
The invention belongs to yolk to evaporate oily preparing technical field, and in particular to a kind of yolk for acid value analysis evaporates the essence of oil
Method processed.
Background technology
It is the oily liquids refined after yolk high-temperature retorting that yolk, which evaporates oil, and modern age evaporates the main component state in oil about yolk
Interior foreign countries have carried out many researchs and have found the biology contained by it especially when exploring the cardiac stimulant ingredient of egg " sustainability of making charcoal " object
Alkali composition harman arabine etc. has antibacterial activity, this evaporates the tinea class skin disease that oily clinic is mainly used for caused by treating fungi, wet with yolk
The diseases such as rash, burn, varicose ulcer are consistent.Although traditional concocting method that yolk evaporates oil is simple, have 1400 in China
History for many years, but be also also easy to produce strong carcinogen BaP simultaneously processing, color is deep, stink is abnormal, make its apply and
It is very limited in related quality analysis.It is carried out further therefore, it is necessary to evaporate oil to the yolk for processing gained through high temperature
It is refined.
The new process that yolk evaporates oil is devised using the methods of microwave method, vacuum distillation.But these methods, which exist, to be changed
The disadvantages such as traditional processing condition, subtractive process are complicated, product purity is low.In addition, the yolk after high-temperature process evaporates oily color darkly
Color, when acid value is analyzed, color judges very difficult.The current acid value of lipids that measures is mainly national standard (GB/T5009.37-2003)
Defined method.The method judges to calculate acid value size by the color of titration end-point, due to the pigment of itself in dark grease
The judgement of titration end-point color is influenced, therefore this method has some limitations.Yolk, which evaporates, contains aliphatic acid and phosphatide in oil,
It is easier to emulsify, also accurate judgement is made to have difficulties using demulsification technology.Supercritical carbon dioxide extraction method utilizes nontoxic
Free of contamination carbon dioxide can be to complicated component by adjusting the operating parameters such as temperature, pressure and flow as Extraction solvent
Mixture extract and detach, have the characteristics that simple for process, effective component extraction rate is high, can solve the above problems.
Invention content
The present invention evaporates in oil that strong carcinogen BaP content is high, color with oil color is difficult to carry out deeply to solve current yolk
The problem of acid value is analyzed, provides a kind of process for purification for being used for the yolk that acid value is analyzed and evaporating oil, and this method uses overcritical two
Carbonoxide extractive technique, evaporates oil to the yolk that high-temperature process destructive distillation obtains and extracts refined, refined yolk and evaporate in oil and cause by force
Cancer substance BaP content significantly reduces, of light color rich in active ingredients substances such as alkaloids, and Product Safety is high.
The present invention is realized by following technical solution：A kind of yolk for acid value analysis evaporates the process for purification of oil, including
Following steps：
（1）Thick yolk, which evaporates, is added adsorbent in oil：It takes the yolk of 250~350 DEG C of high-temperature retortings to evaporate oil, egg is added wherein
Huang evaporates 1~4% adsorbent of weight of oil, and 60~100 DEG C stir evenly, and stands to room temperature；
（2）By step（1）The yolk added with adsorbent of middle acquisition evaporates oil and is added in supercritical carbon dioxide extraction kettle, adjusts
Section extraction kettle temperature degree is 40~55 DEG C, and pressure is 18~55Mpa, CO2Flow be 0.5~10Kg/h, separating still pressure 8~
12Mpa, 60~75 DEG C of separating still temperature, extraction obtain refined yolk and evaporate oil.
Step（1）Described in adsorbent be activated carbon, AB-8 types macroporous absorbent resin or Silon.
The refined yolk obtained evaporates application of the oil as standard items in acid value analysis.
The present invention evaporates oil for raw material with the yolk obtained by high temperature, and adsorbent is added（Activated carbon, AB-8 type macroporous absorbent resins
Or Silon）It is placed it in again in supercritical carbon dioxide extraction element after absorption, adjusts extracting parameter, obtain refined yolk
Evaporate oil product.It is yellow to light yellow that the refined yolk obtained, which evaporates oily color, and grease is rich in unsaturated fatty acid content
65.0~75.0%；Grease Harmane alkaloids content rises to 0.035~0.053%, harmful components Benzpyrene content
It may decrease to 0.010~0.019%.Product includes Harmane and insatiable hunger rich in benefit materials as evaporating oil phase with traditional yolk
And aliphatic acid, and harmful substance BaP removal rate is high；Color with oil color is shallow, can be used for acid value analysis, thus quality is high, safety
Good, modern process that oil can be evaporated for yolk provides strong support.
Gained yolk of the invention evaporates that the alkaloids species composition such as oily Harmane is more, and wherein Harmane content is high, insatiable hunger
With content of fatty acid height.Present invention process is simple, and product colour is shallow, in yellow to light yellow, also can be used for dark colour yolk
Evaporate the acid value analysis of oil.
Description of the drawings
Fig. 1 evaporates harman arabine alkali high-efficiency liquid chromatogram in oil by the refined yolk that the embodiment of the present invention 1 obtains；Fig. 2 is
The refined yolk that the embodiment of the present invention 1 is obtained evaporates BaP high-efficient liquid phase chromatogram in oil；Fig. 3 is 1 institute of the embodiment of the present invention
The refined yolk obtained evaporates aliphatic acid gas chromatogram in oil, in figure：4.2min-5.4min is palmitic acid, 5.4min-6.1min
For palmitoleic acid, 7.6min-9.0min is stearic acid, and 9.0min-11.1min is oleic acid, and 11.1min-12.9min is sub- oil
Acid.
Specific implementation mode
Embodiment 1：A kind of yolk for acid value analysis evaporates the process for purification of oil, includes the following steps：
（1）It is that the black yolk of 250 DEG C of acquisitions evaporates oily 39g to take heating temperature, and activated carbon 0.39g, 60 DEG C of stirrings are added
5min is stood spare to room temperature；
（2）By step（1）The yolk added with activated carbon of sorbent of middle acquisition evaporates oil and supercritical carbon dioxide extraction is added
In kettle, it is 40 DEG C to adjust extraction kettle temperature degree, and extraction pressure is 55Mpa, CO2Flow is 0.5Kg/h, separating still pressure 12Mpa, is divided
75 DEG C from kettle temperature degree, 1.5h is extracted, the yolk for obtaining yellow evaporates oily 23g.
Embodiment 2：A kind of yolk for acid value analysis evaporates the process for purification of oil, includes the following steps：
（1）It is that the black yolk of 350 DEG C of acquisitions evaporates oily 35g to take heating temperature, and activated carbon 1.4g, 80 DEG C of stirrings are added
5min is stood spare to room temperature；
（2）By step（1）The yolk added with activated carbon of sorbent of middle acquisition evaporates oil and supercritical carbon dioxide extraction is added
In kettle, it is 55 DEG C to adjust extraction kettle temperature degree, and extraction pressure is 45Mpa, CO2Flow is 10Kg/h, separating still pressure 8Mpa, separation
Kettle temperature 60 C, extracts 1.5h, and the yolk for obtaining yellow evaporates oily 25g.
Embodiment 3：A kind of yolk for acid value analysis evaporates the process for purification of oil, includes the following steps：
（1）It is that the black yolk of 280 DEG C of acquisitions evaporates oily 45g to take heating temperature, and activated carbon 1.5g, 100 DEG C of stirrings are added
5min is stood spare to room temperature；
（2）By step（1）The yolk added with activated carbon of sorbent of middle acquisition evaporates oil and supercritical carbon dioxide extraction is added
In kettle, it is 45 DEG C to adjust extraction kettle temperature degree, and extraction pressure is 18Mpa, CO2Flow is 5Kg/h, separating still pressure 10Mpa, separation
65 DEG C of kettle temperature degree extracts 1.5h, obtains light yellow clear yolk and evaporate oily 36g.
Embodiment 4：Specific method such as embodiment 3, it is AB-8 type macroporous absorbent resins only to change adsorbent, is obtained light yellow
Clear yolk evaporates oily 36g.
Embodiment 5：Specific method such as embodiment 3, it is Silon only to change adsorbent, obtains light yellow clear yolk
Evaporate oily 35g.
Comparative example 1：100.0g egg yolk powder is added in 1000mL flasks, installs reflux, and heating temperature is arranged
280 DEG C, time 1h is added, black non transparent yolk is collected by filtration while hot after reaction and evaporates oily 40g.
Comparative example 2：It takes 1 yolk of comparative example to evaporate oily 40g, is added in Supercritical carbon dioxide kettle, adjust Extracting temperature 45
DEG C, extraction pressure is 18Mpa, CO2Flow is 5Kg/h, separating still pressure 10Mpa, 65 DEG C of separating still temperature, extracts 1.5h, obtains
Oily 38g is evaporated to light yellow clear yolk.
Above-mentioned gained egg oil measures insatiable hunger through liquid chromatography for measuring Harmane and Benzpyrene content, gas chromatography
And acid content, determination of acid-basetitration acid value, related main physical and chemical index are shown in Table 1.
The different yolk of table 1 evaporate main physical and chemical index in oil samples
As seen from the above table, after in the embodiment of the present invention by refining, yolk evaporates oily harmful components BaP content and declines, benzene
And pyrene is removed rate and at least can reach 62.7%；And main active Harmane and unsaturated fatty acid content are improved,
Wherein Harmane content increases to 0.050% by 0.020% highest, reaches one times or more.Since product colour is shallow, relative to than
Compared with 1 color of example deeply and for can not measuring, acid value is easy detection determination after refining, therefore product leading indicator is controllable, quality peace
Entirely.
Experimental example 1：Yolk evaporates oily main component detection method
It is measured 1. yolk evaporates Harmane in oil：
The preparation of Harmane test solution：1 egg oil of embodiment, 2.5 g accurately is weighed, is put into after weighed with plug
In the conical flask of lid, the ether dissolution of 25 mL is added, 5% 25 mL of hydrochloric acid solution separatory funnel extractions 3 times are added, merge
It is evaporated with thermostat water bath after sour water layer, with being moved in 50 mL volumetric flasks after a small amount of methanol dissolving, last methanol constant volume is put
Enter refrigerator to save backup.
3000 high performance liquid chromatographs of Dai Anyou, chromatographic column：Yi Lite C18 columns (4.6 mm × 250 mm, 5 μm)；Flowing
0.025 mol phosphoric acid triethylamines of phase-methanol (80: 20 )；280 nm of Detection wavelength；Flow velocity l mL/min；Sample size 10
µL；40 DEG C of column temperature.
The making of the standard curve of Harmane and the foundation of regression equation：It is dry to perseverance through 80 DEG C that precision weighs 20 mg
The harman arabine standard items of weight, it is titer to add methanol and 50 mL of constant volume.Precision measures 2.0 μ L, 4.0 μ L, 6.0 μ L, 8.0
μ L, the 10.0 μ L titers, the peak area of Harmane is measured according to chromatographic condition, standard curve is drawn, with Harmane
Reference substance sample size is abscissa X, and integrating peak areas value is ordinate Y, obtains following regression equation：Y=20.526X-
0.1203, R2=0.9996.Harmane content is in good linear relationship with its peak area in 0.08-0.40 μ g ranges.Institute
High-efficient liquid phase chromatogram is obtained as Fig. 1, Harmane retention time is 28.180min in figure.
2. yolk evaporates the measurement of BaP in oil：
The preparation of BaP test solution：Yolk prepared by Example 1 evaporates oil samples 5g, accurately weighed postposition tool
It fills in conical flask, 100mL methanol is added, is extracted respectively 3 times with 50mL hexamethylenes, merge and be evaporated in hexamethylene stratification evaporating dish,
It is moved in 50mL volumetric flasks after a small amount of methanol is added, adds methanol to scale, shake up, stood, solution is through miillpore filter (0.45nm)
Filtration, it is spare.
It is prepared by BaP reference substance solution：Precision measures 50 μ g of BaP reference substance, adds 1.00mL Chromatographic Pure Methanols
Shake up the reference substance solution to get 0.0482mg/mL.
3000 high performance liquid chromatographs of Dai Anyou, chromatographic column C18 reverse-phase chromatographic columns（6.0mm × 150mm, 5um) mobile phase:
Methanol -0.025mol/L phosphoric acid triethylamines (90:10)；Detection wavelength：264nm, flow velocity:LmL/min, column temperature:40 DEG C, theoretical tower
Plate number is calculated by BaP peak should be not less than 2000.BaP high-efficient liquid phase chromatogram is Fig. 2, and BaP retention time is in figure
13.417min。
3. yolk evaporates the measurement that aliphatic acid forms in oil：
Yolk evaporates oily esterification：It takes the yolk prepared by 50 mg embodiments 1 to evaporate oil samples, is placed in tool plug test tube, adds
Enter 2% 0.5 mL of sodium methoxide solution, react at room temperature 30 min, 10% acetic acid aqueous solution is added, shakes up, adds 1 mL n-hexanes
Extraction, takes 1 μ L sample introductions of n-hexane layer.
Chromatographic condition：Chromatographic column is 20% DEGS packed columns of stainless steel（1.2 m×3mm）, Chromosorb.WAW 80/
100 mesh carriers, 250 DEG C of vaporizing chamber, 190 DEG C of column temperature room, 250 DEG C of FID sensing chamber, 35 mL/min of hydrogen flowing quantity, nitrogen flow 45
ML/min, 400 mL/min of air mass flow.Chromatographic work station：N3000.Fatty acid methyl ester is qualitative true with base peak retention time
Fixed, aliphatic acid composition is measured with its peak area normalization method.The aliphatic acid gas chromatogram obtained is Fig. 3.
4. yolk evaporates the measurement of acid value in oil：
This process for purification measures yolk and evaporates the free acid recovering rate of oil：Specific method such as embodiment 3, it is only same in addition activated carbon
When be added 98% standard oleic acid 0.283g of purity, obtain light yellow clear yolk and evaporate oily 36g；From about 2.0g samples are wherein taken, set
In 150 mL triangular flasks, neutral 95% ethyl alcohol is added：Ether（Volume ratio is 1:2）1% phenol of 2-3 drops is added in 50 mL of mixed solvent
Phthalein ethyl alcohol indicator is titrated after shaking up with the standard K OH solution of 0.100mmol/L, solution colour become it is micro- it is red after 30s do not take off into
Titration end-point calculates acid value, and is converted into oleic acid quality, calculates sample recovery rate of this method to free acid in grease.
Saturated sodium-chloride breaking method measures yolk and evaporates the free acid recovering rate of oil：Described in concrete operations process for purification as above,
The only saturated nacl aqueous solution 20mL before titration.
No additive process method measures yolk and evaporates the free acid recovering rate of oil：Concrete operations are according to national standard (GB/T5009.37-
2003) method as defined in carries out, and has no other special changes.
1-3 samples are to be carried out using this process for purification in following table；4-5 samples are 1 oil sample of comparative example using saturation chlorine
Change sodium breaking method to carry out；No. 6 samples are to 1 oil sample of comparative example without additional treatments.
The different yolk of table 2 evaporate the sample recovery rate of free acid in oil
As can be seen from Table 2, the sample recovery rate difference that the yolk of distinct methods processing evaporates free acid in oil is apparent.Due to yolk
It is pitch black and containing the easy emulsified component such as phosphatide to evaporate oily color, is difficult to judge end using traditional national standard method of no additional treatments
Point can not detected the free acid of addition；And even if using saturated sodium-chloride breaking method free acid sample recovery rate
It is relatively low；But use this process for purification free acid be added yolk evaporate then obtained in oil 95% or more the rate of recovery, pass through calculating
Also it can be seen that its relative standard deviation value is less than 2%.This method is without adding demulsifier, and titration end-point is clear and legible, and free acid adds
The sample rate of recovery is high, accurate and easy, and oil or other compounds such as aliphatic acid or mixture can be evaporated as jet black colors yolk
Acid value detection effective means promote the use of.
Claims (2)
1. a kind of yolk for acid value analysis evaporates the process for purification of oil, it is characterised in that：Include the following steps：
（1）Thick yolk, which evaporates, is added adsorbent in oil：It takes the yolk of 250~350 DEG C of high-temperature retortings to evaporate oil, yolk is added wherein and evaporates
1~4% adsorbent of weight of oil, 60~100 DEG C stir evenly, and stand to room temperature；
（2）By step（1）The yolk added with adsorbent of middle acquisition evaporates oil and is added in supercritical carbon dioxide extraction kettle, and adjusting carries
It is 40~55 DEG C to take kettle temperature degree, and pressure is 18~55Mpa, CO2Flow is 0.5~10Kg/h, separating still 8~12Mpa of pressure, is divided
60~75 DEG C from kettle temperature degree, extraction obtains refined yolk and evaporates oil.
2. a kind of yolk for acid value analysis according to claim 1 evaporates the process for purification of oil, it is characterised in that：Step
（1）Described in adsorbent be activated carbon, AB-8 types macroporous absorbent resin or Silon.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5480402A (en) * | 1977-12-06 | 1979-06-27 | Fujinaga Seiyaku Kk | Improved pharmaceutical tar agent and production 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 |
| CN101015583A (en) * | 2006-02-10 | 2007-08-15 | 重庆华邦制药股份有限公司 | Refining method for black soya bean distillation oil |
| CN103013653A (en) * | 2012-12-28 | 2013-04-03 | 广州白云山汉方现代药业有限公司 | Preparation method of refined egg oil |
-
2015
- 2015-08-10 CN CN201510482721.5A patent/CN105132152B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5480402A (en) * | 1977-12-06 | 1979-06-27 | Fujinaga Seiyaku Kk | Improved pharmaceutical tar agent and production 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 |
| CN101015583A (en) * | 2006-02-10 | 2007-08-15 | 重庆华邦制药股份有限公司 | Refining method for black soya bean distillation oil |
| CN103013653A (en) * | 2012-12-28 | 2013-04-03 | 广州白云山汉方现代药业有限公司 | Preparation method of refined egg oil |
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