CN105105118A - Method for preparing sea cucumber intestine lipid rich in EPA - Google Patents
Method for preparing sea cucumber intestine lipid rich in EPA Download PDFInfo
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- CN105105118A CN105105118A CN201510551605.4A CN201510551605A CN105105118A CN 105105118 A CN105105118 A CN 105105118A CN 201510551605 A CN201510551605 A CN 201510551605A CN 105105118 A CN105105118 A CN 105105118A
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Abstract
The invention discloses a method for preparing sea cucumber intestine lipid rich in EPA. The method comprises the following steps: pre-treating sea cucumber intestines, homogenizing so as to obtain sea cucumber intestine homogenate, adding an McIIvaines buffer liquid of a sodium hydrogen phosphate-citric acid buffer solution into the sea cucumber intestine homogenate, subsequently adding a chloroform/methanol solution, performing vibration extraction, putting the mixed liquid into a centrifuge to separate the lipid layer, and performing nitrogen-blowing, thereby obtaining the sea cucumber intestine lipid. The method has the characteristics of simple process, simple operation and high efficiency, the conditions of the extraction method are gentle, original physiological activators in sea cucumber intestine lipid can be maintained to the maximum extent, and a product has nutritional and functional properties.
Description
Technical field
The present invention relates to a kind of preparation method of sea cucumber intestine lipid, more particularly, relate to a kind of preparation method being rich in EPA sea cucumber intestine lipid.
Background technology
Sea cucumber intestine is the accessory substance in Holothurian machining process, its fat content can reach about 7.80 ± 0.49% (with dry weight basis), unrighted acid relative amount reaches about 84.62%, and the content of EPA is higher, therefore, sea cucumber intestine lipid is the good source of polyunsaturated fatty acid, has good development prospect in healthy food field.In China, sea cucumber intestine is many, and lost utilization rate as discarded object extremely low, causes the wasting of resources and environmental pollution.
About the bibliographical information of sea cucumber intestine grease, mainly concentrate on and lipid content is studied.Korea S scholar joins the Red sea from Yu Ling island and Dokdo and Holothuria atra crude fat measures, and result shows that wall of sea cucumber Stichopus japonicus and internal organ crude fat content account for 0.14 ~ 2.12%.But, relevant report be there is not yet for the preparation of grease in sea cucumber intestine.
This patent adopts McIIvaines buffer solution in conjunction with organic solvent in the method extracting sea cucumber intestine grease, there is technique simple, easy to operate, the feature that efficiency is high, extracting method mild condition, can preserve original physiological activator in sea cucumber intestine grease to greatest extent, make product have trophism and functional concurrently, the exploitation for sea cucumber intestine resource have great importance.
Summary of the invention
In sea cucumber intestine, unrighted acid relative amount is up to 84.62%, and the content of EPA is higher, and in sea cucumber intestine, the Application way of preparing of grease there is no report.The preparation problem of grease in unresolved sea cucumber intestine, the invention provides a kind of preparation method being rich in EPA sea cucumber intestine lipid, and the method for the invention has mild condition, feature that production efficiency is high, and the sea cucumber intestine lipid obtained by this method is rich in EPA.
A kind of preparation method being rich in EPA sea cucumber intestine lipid of the present invention, is characterized in that, comprise the steps:
S1, sea cucumber intestine pretreatment, homogenate, obtains sea cucumber intestine homogenate;
S2, in sea cucumber intestine homogenate described in step S1, add McIIvaines buffer solution, mix, obtain sea cucumber intestine mixed liquor; Described McIIvaines pH of buffer is 3 ~ 8;
S3, to chloroform/methanol solution concussion extraction 1 ~ 2min in sea cucumber intestine mixed liquor described in step S2, obtain sea cucumber intestine extract; It is 2:1 that described chloroform/methanol Chlorine in Solution is imitated with the volume ratio of methyl alcohol;
S4, by centrifugal for sea cucumber intestine extract described in step S3, collect lower floor chloroform layer solution; Described chloroform layer solution is sea cucumber intestine lipid after nitrogen blows;
The volume ratio of described sea cucumber intestine homogenate, McIIvaines buffer solution and chloroform/methanol solution is 1:1 ~ 3:1 ~ 3.
Under preferred embodiment, McIIvaines buffer solution described in step S2 is sodium hydrogen phosphate-citric acid solution.Under optimum way, McIIvaines pH of cushioning fluid described in step S2 is 3; The volume that described McIIvaines buffer solution adds is 3 times of sea cucumber intestine homogenate described in step S1.
Under preferred embodiment, described in step S3 after adding chloroform/methanol solution concussion extraction, then add chloroform concussion extraction 1 ~ 2min; The volume ratio of described sea cucumber intestine homogenate and chloroform/methanol solution, chloroform is 1:1 ~ 3:1 ~ 3.Under optimum way, step S3 is the concussion 1min first adding chloroform/methanol solution, then adds chloroform concussion 1min; The volume ratio of described sea cucumber intestine homogenate and chloroform/methanol solution, chloroform is 1:3:1.
Under preferred embodiment, the condition of centrifugation described in step S4 is the centrifugal 5 ~ 10min of 2000 ~ 5000r/min.
Technological innovation of the present invention is:
1, improve the utilization rate of Holothurian machining byproduct in process thing, the active material making it contain fully is developed, and decreases the pollution to environment simultaneously.Sea cucumber intestine lipid after processing process is rich in EPA, can be used as function base-material for developing several functions product.
2, lixiviate grease process temperature of the present invention is low, can preserve more original physiological activators in sea cucumber intestine lipid to greatest extent, makes product have trophism and functional concurrently;
3, the operating process that the present invention relates to is simple, and do not need complicated equipment, sea cucumber intestine lipids extraction rate is high, reaches 5.4%, EPA relative amount and reaches 30.97%, improve production efficiency, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the recovery rate that different pH extracts sea cucumber intestine lipid.
Detailed description of the invention
The concrete steps of the inventive method are:
S1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
PH3 is added, the McIIvaines buffer solution (1 ~ 3:1) of the sodium hydrogen phosphate-citric acid solution of pH4, pH5, pH6, pH7, pH8 in S2, sea cucumber intestine homogenate;
Add chloroform/methanol (2:1) the solution concussion 1 ~ 2min of 1 ~ 3 times of volume in S3, step S2 gained mixed liquor, and then add the chloroformic solution concussion 1 ~ 2min of 1 ~ 3 times of volume;
S4, step S3 gained mixed liquor put into centrifuge with the centrifugal 5 ~ 10min of 2000 ~ 5000r/min, after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and are transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows.
Under above-mentioned preferred embodiment, optimal situation is:
In step S2, the McIIvaines pH of cushioning fluid of sodium hydrogen phosphate-citric acid solution is 3, and adding proportion is 1:3.
First add the concussion 1min of 3 times of volume of chloroform/methyl alcohol (2:1) solution in step S3, and then add the chloroformic solution concussion 1min of 1 times of volume.
Embodiment 1
1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
2, sea cucumber intestine homogenate 1ml, adds the McIIvaines buffer solution 3ml of pH3 sodium hydrogen phosphate-citric acid solution;
3, add chloroform/methanol (2:1) the solution concussion 2min of 3ml in mixed liquor, and then add the chloroformic solution concussion 1min of 1ml;
4, mixed liquor puts into centrifuge with the centrifugal 10min of 4000r/min, and after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and be transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows, extraction rate reached 5.4%, EPA relative amount is 31.13%.
Embodiment 2
1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
2, sea cucumber intestine homogenate 1ml, adds the McIIvaines buffer solution 3ml of pH4 sodium hydrogen phosphate-citric acid solution;
3, add chloroform/methanol (2:1) the solution concussion 2min of 2ml in mixed liquor, and then add the chloroformic solution concussion 1min of 1ml;
4, mixed liquor puts into centrifuge with the centrifugal 10min of 2000r/min, and after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and be transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows, extraction rate reached 4.3%, EPA relative amount is 29.87%.
Embodiment 3
1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
2, sea cucumber intestine homogenate 1ml, adds the McIIvaines buffer solution 2ml of pH5 sodium hydrogen phosphate-citric acid solution;
3, add chloroform/methanol (2:1) the solution concussion 2min of 2ml in mixed liquor, and then add the chloroformic solution concussion 1min of 2ml;
4, mixed liquor puts into centrifuge with the centrifugal 5min of 5000r/min, and after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and be transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows, extraction rate reached 4.1%, EPA relative amount is 26.02%.
Embodiment 4
1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
2, sea cucumber intestine homogenate 1ml, adds the McIIvaines buffer solution 3ml of pH6 sodium hydrogen phosphate-citric acid solution;
3, add chloroform/methanol (2:1) the solution concussion 1min of 2ml in mixed liquor, and then add the chloroformic solution concussion 2min of 1ml;
4, mixed liquor puts into centrifuge with the centrifugal 10min of 3000r/min, and after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and be transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows, extraction rate reached 3.3%, EPA relative amount is 28.86%.
Embodiment 5
1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
2, sea cucumber intestine homogenate 1ml, adds the McIIvaines buffer solution 1ml of pH7 sodium hydrogen phosphate-citric acid solution;
3, add chloroform/methanol (2:1) the solution concussion 2min of 2ml in mixed liquor, and then add the chloroformic solution concussion 1min of 3ml;
4, mixed liquor puts into centrifuge with the centrifugal 10min of 4000r/min, and after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and be transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows, extraction rate reached 2.6%, EPA relative amount is 30.24%.
Embodiment 6
1, get fresh sea cucumber intestine, remove silt in intestines, clean with deionized water rinsing, homogenate obtains sea cucumber intestine homogenate;
2, sea cucumber intestine homogenate 1ml, adds the McIIvaines buffer solution 1ml of pH8 sodium hydrogen phosphate-citric acid solution;
3, add chloroform/methanol (2:1) the solution concussion 2min of 1ml in mixed liquor, and then add the chloroformic solution concussion 2min of 3ml;
4, mixed liquor puts into centrifuge with the centrifugal 5min of 3000r/min, and after the centrifugal layering of sample mix liquid, draw lower floor's chloroform layer solution and be transferred in glass tube, namely obtain sea cucumber intestine grease after nitrogen blows, extraction rate reached 2.9%, EPA relative amount is 29.71%.
Table 1 is the impact of pH on EPA in sea cucumber intestine lipid, and when the pH of McIIvaines buffer solution is 3, the EPA relative amount of sea cucumber intestine lipid is the highest, reaches 31.13%, and along with the rising of pH, in lipid, EPA relative amount presents the trend first reducing and raise afterwards.When the pH of McIIvaines buffer solution is 5, in sea cucumber intestine lipid, EPA relative amount is minimum is 26.02%; When the pH of McIIvaines buffer solution rises to 6,7 and 8, in sea cucumber intestine lipid, EPA relative amount gos up gradually.
Table 1
The state extracting sea cucumber intestine lipid under condition of different pH is different, and when cushioning liquid pH is 3, the color of lipid layer is the darkest, and emulsion layer is the thinnest.In the scope of pH4 ~ 8, along with the raising gradually of pH, lipid layer color shoals gradually, and emulsion layer increases gradually.
PH is on the impact of sea cucumber intestine lipids extraction as seen from Figure 1, and when the pH of McIIvaines buffer solution is 3, the recovery rate of sea cucumber intestine lipid is the highest, reaches 5.40 ± 0.15%, is increased to neutrality along with pH, and lipids extraction rate declines gradually.When the pH of McIIvaines buffer solution is 4 and 5, sea cucumber intestine recovery rate has no significant difference (p>0.05); When the pH of McIIvaines buffer solution rises to 6 and 7, sea cucumber intestine recovery rate significantly declines, and reaches minimum.When the pH of McIIvaines buffer solution is 8, comparatively pH7 recovery rate slightly gos up.
The above; be only the present invention's preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (7)
1. be rich in a preparation method for EPA sea cucumber intestine lipid, it is characterized in that, comprise the steps:
S1, sea cucumber intestine pretreatment, homogenate, obtains sea cucumber intestine homogenate;
S2, to McIIvaines buffer solution in sea cucumber intestine homogenate described in step S1, to mix, obtain sea cucumber intestine mixed liquor; Described McIIvaines pH of buffer is 3 ~ 8;
S3, to chloroform/methanol solution concussion extraction 1 ~ 2min in sea cucumber intestine mixed liquor described in step S2, obtain sea cucumber intestine extract; It is 2:1 that described chloroform/methanol Chlorine in Solution is imitated with the volume ratio of methyl alcohol;
S4, by centrifugal for sea cucumber intestine extract described in step S3, collect lower floor chloroform layer solution; Described chloroform layer solution is sea cucumber intestine lipid after nitrogen blows;
The volume ratio of described sea cucumber intestine homogenate, McIIvaines buffer solution and chloroform/methanol solution is 1:1 ~ 3:1 ~ 3.
2. be rich in the preparation method of EPA sea cucumber intestine lipid according to claim 1, it is characterized in that, McIIvaines buffer solution described in step S2 is sodium hydrogen phosphate-citric acid solution.
3. be rich in the preparation method of EPA sea cucumber intestine lipid according to claim 2, it is characterized in that, McIIvaines pH of cushioning fluid described in step S2 is 3.
4. be rich in the preparation method of EPA sea cucumber intestine lipid according to claim 3, it is characterized in that, the volume that described in step S2, McIIvaines buffer solution adds is 3 times of sea cucumber intestine homogenate described in step S1.
5. be rich in the preparation method of EPA sea cucumber intestine lipid according to claim 1, it is characterized in that, described in step S3 after adding chloroform/methanol solution concussion extraction, then add chloroform concussion extraction 1 ~ 2min; The volume ratio of described sea cucumber intestine homogenate and chloroform/methanol solution, chloroform is 1:1 ~ 3:1 ~ 3.
6. be rich in the preparation method of EPA sea cucumber intestine lipid according to claim 5, it is characterized in that, step S3 is the concussion 1min first adding chloroform/methanol solution, then adds chloroform concussion 1min; The volume ratio of described sea cucumber intestine homogenate and chloroform/methanol solution, chloroform is 1:3:1.
7. be rich in the preparation method of EPA sea cucumber intestine lipid according to claim 1, it is characterized in that, the condition of centrifugation described in step S4 is the centrifugal 5 ~ 10min of 2000 ~ 5000r/min.
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| CN109793150A (en) * | 2019-03-02 | 2019-05-24 | 大连棒棰岛海产股份有限公司 | Sea cucumber intestine extract solid seasoning and its preparation method |
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| JP2002501030A (en) * | 1998-01-21 | 2002-01-15 | ピーター・ドナルド・コリン | Sea cucumber carotenoid lipid fraction product and method of using same |
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Cited By (1)
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| CN109793150A (en) * | 2019-03-02 | 2019-05-24 | 大连棒棰岛海产股份有限公司 | Sea cucumber intestine extract solid seasoning and its preparation method |
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