CN102876447A - Goose fat liver oil extracting method - Google Patents
Goose fat liver oil extracting method Download PDFInfo
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- CN102876447A CN102876447A CN2012103956535A CN201210395653A CN102876447A CN 102876447 A CN102876447 A CN 102876447A CN 2012103956535 A CN2012103956535 A CN 2012103956535A CN 201210395653 A CN201210395653 A CN 201210395653A CN 102876447 A CN102876447 A CN 102876447A
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- 210000004185 liver Anatomy 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000000605 extraction Methods 0.000 claims abstract description 69
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 239000000284 extract Substances 0.000 claims abstract description 15
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract 6
- 239000003208 petroleum Substances 0.000 claims abstract 3
- 239000000203 mixture Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 150000004670 unsaturated fatty acids Chemical class 0.000 abstract description 6
- 235000021122 unsaturated fatty acids Nutrition 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 208000004930 Fatty Liver Diseases 0.000 abstract 3
- 206010019708 Hepatic steatosis Diseases 0.000 abstract 3
- 208000010706 fatty liver disease Diseases 0.000 abstract 3
- 231100000240 steatosis hepatitis Toxicity 0.000 abstract 3
- 239000007788 liquid Substances 0.000 description 17
- 230000008569 process Effects 0.000 description 16
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- 230000003993 interaction Effects 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000004519 grease Substances 0.000 description 6
- 235000014113 dietary fatty acids Nutrition 0.000 description 5
- 239000000194 fatty acid Substances 0.000 description 5
- 229930195729 fatty acid Natural products 0.000 description 5
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- 238000005360 mashing Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
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- 239000005642 Oleic acid Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
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- 229960004232 linoleic acid Drugs 0.000 description 1
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- 235000016709 nutrition Nutrition 0.000 description 1
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- 230000000050 nutritive effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
本发明涉及一种鹅肥肝油提取方法，包括有如下的步骤：1)鹅肥肝浆液的制备；2）鹅肥肝油提取：将浆液和石油醚混合后用超声波进行提取，提取完成后，将提取液进行离心，取上清液进行过滤，采用真空旋转蒸发仪去除滤液中提取剂，再干燥获得鹅肥肝油产品；其中超声提取的条件：提取温度为10℃～50℃、提取时间为5min～25min、提取功率为200W～500W。本发明采用超声波辅助提取的方法提取鹅肥肝油，充分利用超声波的空化作用、机械作用、热效应三大效应的优点，不仅大大缩短了提取时间，还在一定程度上降低了提取温度，提高了提取效果，有效防止不饱和脂肪酸的氧化，填补了该领域的空白，为鹅肥肝油的提取探索出一种新的方法，具有重要的经济和社会价值。
The invention relates to a method for extracting goose fatty liver oil, comprising the following steps: 1) preparation of goose fatty liver slurry; 2) extraction of goose fatty liver oil: mixing the slurry with petroleum ether and then extracting it with ultrasonic waves; after the extraction is completed, the The extract is centrifuged, the supernatant is filtered, and the extractant in the filtrate is removed by a vacuum rotary evaporator, and then dried to obtain the foie gras oil product; the conditions for ultrasonic extraction: the extraction temperature is 10°C to 50°C, and the extraction time is 5 minutes ~25min, extraction power is 200W~500W. The invention adopts the ultrasonic-assisted extraction method to extract goose liver oil, and fully utilizes the advantages of the three major effects of ultrasonic cavitation, mechanical action and thermal effect, not only greatly shortens the extraction time, but also reduces the extraction temperature to a certain extent, and improves the extraction efficiency. The extraction effect can effectively prevent the oxidation of unsaturated fatty acids, which fills the gap in this field and explores a new method for the extraction of foie gras oil, which has important economic and social value.
Description
Technical field:
The invention belongs to grease extractive technique field, be specifically related to a kind of fat goose liver oil extracting method.
Background technology:
Fat goose liver is to adopt specific feed and compounding process that goose is carried out forced-feeding and the liver that generates; The fat goose liver main active substances is foie gras oil, and it is rich in the nutritive ingredients such as unsaturated fatty acids, Yelkin TTS, triglyceride level and various trace elements of needed by human body.Wherein unsaturated fatty acid content is very high, have delay senility, the effect such as blood fat reducing and vessel softening; And contained linolic acid is indispensable fatty acid, and human body can not self synthesize, and can only lean on from ingestion of food, and therefore, the extraction of fat goose liver oil has important social effect to the needs that satisfy the different consumer groups.But the extracting method length consuming time of present animal product grease, temperature is high, is easy to make the unsaturated fatty acids generation oxidation that contains, and the nutrition of grease and economic worth are reduced.Therefore, be necessary to provide a kind of extracting method of more effective fat goose liver oil.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of fat goose liver oil namely adopts the method for ultrasonic-assisted extraction to prepare fat goose liver oil, to fill up the at present blank in this field.
The applicant is devoted to study the best approach of ultrasonic extraction method fat goose liver oil always, by long research, through the screening to solid-liquid ratio, ultrasonic power, ultrasonic treatment time and four factors for the treatment of temp in the supersound process process, determine the optimum process condition that the ultrasonic-assisted extraction method is extracted fat goose liver oil.
Fat goose liver oil extracting method of the present invention includes following step:
1) preparation of fat goose liver slurries: fat goose liver is carried out homogenate obtain slurries;
2) fat goose liver oil extracts: will extract with ultrasonic wave after slurries and the sherwood oil mixing; After extraction is finished, extracting solution is carried out centrifugal, get supernatant liquor and filter; Utilize vacuum rotary evaporator to remove extraction agent sherwood oil in the filtrate, the drier fat goose liver oil that obtains; The condition of ultrasonic extraction wherein: extracting temperature and be 10 ℃～50 ℃, extraction time is that 5min～25min, extraction power are 200W～500W.
Above-mentioned slurries and the mass volume ratio of sherwood oil are 1:4～8, are preferably 1:5
The said extracted temperature is preferably 35 ℃, and ultrasonic power is preferably 440W, and extraction time is preferably 11min.
The present invention adopts the method for ultrasonic-assisted extraction to extract fat goose liver oil, take full advantage of the advantage of hyperacoustic cavatition, mechanical effect, heat effect three large effects, not only greatly shortened extraction time, also reduced to a certain extent the extraction temperature, improve extraction effect, prevented the oxidation of unsaturated fatty acids, filled up the blank in this field, explore a kind of new method for the extraction of fat goose liver oil, have important economic society and be worth.
Description of drawings
Fig. 1: interaction response face figure between solid-liquid ratio and the ultrasonic power among the present invention;
Fig. 2: solid-liquid ratio and interaction response face figure between extraction time among the present invention;
Fig. 3: interaction response face figure between solid-liquid ratio and the extraction temperature among the present invention;
Fig. 4: ultrasonic power and interaction response face figure between extraction time among the present invention;
Fig. 5: interaction response face figure between ultrasonic power and the extraction temperature among the present invention;
Fig. 6: interaction response face figure between extraction time and the extraction temperature among the present invention;
Fig. 7: fat goose liver oil standard product gas-chromatography collection of illustrative plates;
Fig. 8: the fat goose liver oil gas phase chromatogram collection of illustrative plates that the present invention extracts.
Embodiment
The present invention adopts the method for ultrasonic extraction to extract fat goose liver oil, select sherwood oil as extraction agent, take the grease extraction yield as index, solid-liquid ratio, ultrasonic treatment time, ultrasonication temperature and ultrasonic power are factor, the test of design response surface, obtain preparing the optimum extraction condition of fat goose liver oil, and the mensuration that fatty acid content in the fat goose liver oil of preparation has been carried out.
The extracting method of fat goose liver oil comprises the steps: among the present invention
1) preparation of fat goose liver slurries: fat goose liver is carried out homogenate obtain slurries;
The fat goose liver sample is pulpous state through tissue mashing machine after smashing to pieces, not only is conducive to fully contacting of sample and extraction agent, and is easy to brokenly in the ultrasonication process, is easier to the release of fat particle, so that extraction effect is better.
2) fat goose liver oil extracts: will extract with ultrasonic wave after slurries and the sherwood oil mixing; After extraction is finished, extracting solution is carried out centrifugal, get supernatant liquor and filter, utilize vacuum rotary evaporator to remove extraction agent in the filtrate, the drier fat goose liver oil that obtains; The condition of supersound extraction wherein: extracting temperature and be 10 ℃～50 ℃, extraction time is that 5min～25min, extraction power are 200W～500W.
With the fat goose liver oil gas chromatography determination fatty acid content that extracts, namely at ambient temperature sample is methylated, and moisture is wherein adsorbed rear use Agilent 7890A gas-chromatography analyze, use fid detector, chromatographic column is the CP-Sil88 Fused-silica capillary column.
Below in conjunction with specific embodiment method of the present invention is described in detail.
Embodiment 1: the screening of ultrasonic extraction method fat goose liver oil top condition
1, the preparation of fat goose liver slurries
To test to cut with fat goose liver mixing uniform fritter, and put into tissue mashing machine and fully smash to pieces and be pulpous state, minute be filled in the different freshness protection packages, and place preserve in the subzero refrigerator below 18 ℃ stand-by.
2, fat goose liver oil extracts
(described solid-liquid ratio refers to the quality of fat goose liver according to solid-liquid ratio, being the mass volume ratio of fat goose liver slurries and extracting solution) ratio of 1:4～8 adds fat goose liver and sherwood oil in the processing cup of ultrasonic extraction instrument, and set to extract temperature be that 10 ℃～50 ℃, extraction time are that 5min～25min, extraction power are 200W～500W, and opening power is carried out ultrasonic extraction.After extraction is finished, extracting solution is filtered behind the centrifugal 10min in supercentrifuge, filtrate under 35 ℃ of conditions after rotary evaporation in vacuo is removed extraction agent, put into the loft drier inner drying to constant weight, and calculate extraction yield.
Optimization for above-mentioned extraction conditions is as follows:
(1) screening of solid-liquid ratio (m:v)
The setting ultrasonic power is 200W, the supersound process time is 10min, and treatment temp is under 20 ℃ the condition, and the ratio of regulating fat goose liver and sherwood oil is that 1:4,1:5,1:6,1:7,1:8 test respectively, measure fat goose liver oil extraction yield, and its solid-liquid ratio is carried out preliminary screening.
(2) screening of ultrasonic power
The setting solid-liquid ratio is 1:5, the supersound process time is 10min, and treatment temp is under 20 ℃ the condition, regulates ultrasonication power and be 100W, 200W, 300W, 400W, 500W tests respectively, measure fat goose liver oil extraction yield, so that its ultrasonic power is carried out preliminary screening.
(3) screening of ultrasonic treatment time
The setting solid-liquid ratio is 1:5, ultrasonic power is 400W, and treatment temp is under 20 ℃ the condition, and the adjusting ultrasonic treatment time is that 5min, 10min, 15min, 20min, 25min test respectively, measure fat goose liver oil extraction yield, so that ultrasonic treatment time is carried out preliminary screening.
(4) screening of ultrasonication temperature
The setting solid-liquid ratio is 1:5, and ultrasonic power is 400W, and the treatment time is 10min, and the adjusting treatment temp is 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃ to be tested respectively, measures fat goose liver oil extraction yield, so that the ultrasonication temperature is carried out preliminary screening.
(5) response surface testing program and result
Table 1 response surface scheme and result
(6) Establishment and analysis of response-surface model
Draw its equation of linear regression after by response surface software design expert 7.0.0 test-results being analyzed as follows:
Y=65.31+1.85A+5.41B+2.39C+0.47D-0.060AB-1.43AC-1.02AD+1.96BC-1.91BD+0.83CD-1.32A
2-8.31B2-2.19C
2-1.35D
2
In the formula: A represents solid-liquid ratio; B represents ultrasonic power; The C supersound process time; D represents the supersound process temperature, and variance analysis, result such as table 2 are carried out in above-mentioned response surface test.
The variance analysis of table 2 response surface
As seen from table, regression model integral body is extremely significantly (P＜0.01), and model loses and intends item is 0.0535＜0.05, does not have the significance impact, illustrates that residual error is caused by random error, and regression equation can replace true point to carry out the analysis of test-results.Model coefficient of determination R
2=0.957, show that model-fitting degree is better, this test of description that can be good.Once item is B on the big or small ordering of test impact〉C〉A〉D, that is: ultrasonic power〉the supersound process time〉solid-liquid ratio〉the supersound process temperature, wherein ultrasonic power has utmost point significance impact (P＜0.01) to test, and supersound process time and solid-liquid ratio have a significant impact (P＜0.05) to test.BC and BD significance are better in mutual, and ultrasonic power and supersound process time are described, the impact of the interaction partners extraction yield of ultrasonic power and treatment temp is larger.Behind design expert 7.0 software analysis, the optimum process condition that draws ultrasonic extraction method fat goose liver oil is: solid-liquid ratio 1:5.0, ultrasonic power are 400W, and extraction time is 11min, extracting temperature is 35 ℃, and the extraction yield of fat goose liver oil is 67.44% with this understanding.For optimal conditions the results detailed in accompanying drawing 1-6.
3, fatty acid content in the gas chromatography determination fat goose liver oil
Take by weighing the 2mg sample, add respectively normal hexane 1.5mL, ethyl acetate 40uL, then add NaOCH
3/ CH
320min methylates under the room temperature condition behind the OH100uL.Place refrigerated tank to leave standstill 10min, add rapidly the oxalic acid of 60 μ L after the taking-up, centrifugal going precipitated, and solution is passed through anhydrous Na SO
4Layer is with absorption moisture wherein.Use Agilent 7890A gas-chromatography to analyze, use fid detector.Gas chromatographic column is the CP-Sil88 Fused-silica capillary column.
Take after measured in the fat goose liver oil that the technique optimized extracts take stearic acid, palmitinic acid, physetoleic acid and oleic acid as main, wherein unsaturated fatty acid content accounts for more than 71% of grease total mass, is higher than 65%～68% of report.See accompanying drawing 7 and accompanying drawing 8 for details.
Embodiment 2: solvent extraction method extracts fat goose liver oil
(1) preparation of fat goose liver slurries: fat goose liver is carried out homogenate obtain slurries;
Adopt the 120g fat goose liver to carry out tissue mashing and process the acquisition slurries, before extracting, be placed on cryopreservation;
(2) fat goose liver oil extracts
Solid-liquid ratio 1:5.0, ultrasonic power are 400W, and extraction time is 11min, and extracting temperature is 35 ℃,
Choosing sherwood oil is extraction agent, and according to the optimal extract process of above-mentioned ultrasonic extraction, namely adds the 600ml sherwood oil in 120g fat goose liver slurries, is that 35 ℃, ultrasonic power are to extract 11min under the constant temperature of 400W in temperature; Extracting solution is carried out centrifugal rear filtration under the 3000r/min condition, filtrate is put into the loft drier inner drying to constant weight behind rotary evaporation, finish extraction.The foie gras oil gas phase chromatography that extracts is measured wherein fatty acid content.And carry out according to the method described above the mensuration of fat goose liver oil extraction yield, and the result shows, the extraction yield of case study on implementation 2 is 45%, far below 67.44% under case study on implementation 1 top condition; Therefore, the extracting method of embodiment 1 is comparatively desirable.
Method of the present invention can be extracted foie gras oil effectively fully, not only can greatly shorten extraction time, can also reduce the extraction temperature, reduces oxidation and the energy expenditure of grease, and technique can be applied to the exploitation of foie gras oil production.
Claims (6)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105494887A (en) * | 2015-12-19 | 2016-04-20 | 仇颖超 | Method for extracting soya bean lecithin from soybean curb residues |
| CN107267276A (en) * | 2017-08-06 | 2017-10-20 | 青岛农业大学 | It is a kind of to digest the method that centrifugal process extracts Goose fat liver oil |
| CN107267277A (en) * | 2017-08-06 | 2017-10-20 | 青岛农业大学 | A kind of duck fatty liver oil and preparation method thereof |
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| CN1900246A (en) * | 2006-07-18 | 2007-01-24 | 唐淮生 | Goose liver oil and goose fat liver oil |
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2012
- 2012-10-17 CN CN2012103956535A patent/CN102876447A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105494887A (en) * | 2015-12-19 | 2016-04-20 | 仇颖超 | Method for extracting soya bean lecithin from soybean curb residues |
| CN107267276A (en) * | 2017-08-06 | 2017-10-20 | 青岛农业大学 | It is a kind of to digest the method that centrifugal process extracts Goose fat liver oil |
| CN107267277A (en) * | 2017-08-06 | 2017-10-20 | 青岛农业大学 | A kind of duck fatty liver oil and preparation method thereof |
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