KR20170069483A - Quality characterization of salmon oil microencapsulated with various wall materials - Google Patents

Quality characterization of salmon oil microencapsulated with various wall materials Download PDF

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Publication number
KR20170069483A
KR20170069483A KR1020150176727A KR20150176727A KR20170069483A KR 20170069483 A KR20170069483 A KR 20170069483A KR 1020150176727 A KR1020150176727 A KR 1020150176727A KR 20150176727 A KR20150176727 A KR 20150176727A KR 20170069483 A KR20170069483 A KR 20170069483A
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KR
South Korea
Prior art keywords
salmon
extraction
salmon oil
oil
fish frame
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KR1020150176727A
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Korean (ko)
Inventor
이원경
민진기
임현정
김민정
박슬기
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주식회사 씨웰
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Priority to KR1020150176727A priority Critical patent/KR20170069483A/en
Publication of KR20170069483A publication Critical patent/KR20170069483A/en

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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2200/00Function of food ingredients
    • A23V2200/20Ingredients acting on or related to the structure
    • A23V2200/224Encapsulating agent
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2250/00Food ingredients
    • A23V2250/18Lipids
    • A23V2250/186Fatty acids
    • A23V2250/1882Polyunsaturated fatty acids
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2250/00Food ingredients
    • A23V2250/20Natural extracts
    • A23V2250/204Animal extracts
    • A23V2250/2042Marine animal, fish extracts
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2300/00Processes
    • A23V2300/10Drying, dehydrating
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2300/00Processes
    • A23V2300/14Extraction
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2300/00Processes
    • A23V2300/31Mechanical treatment
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2300/00Processes
    • A23V2300/38Multiple-step

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The present invention relates to a method for removing salmon, comprising: separating a fish frame of a salmon; Drying and crushing the separated fish frame; Extracting salmon oil from a crushed fish frame using a heating method selected from the group consisting of hot water extraction and organic solvent extraction, or a non-heating method such as supercritical extraction or compression extraction; Spray drying the extracted salmon oil to microencapsulate; And a microcapsule of salmon oil prepared therefrom.

Description

TECHNICAL FIELD The present invention relates to a microencapsulation method of salmon oil and salmon oil microcapsules prepared thereby,

The present invention relates to a microencapsulation method of salmon oil and a salmon oil microcapsule produced thereby, and more particularly, to a microencapsulation method of salmon oil which is low in fat acidity and maintains proper quality even when stored for a long time, Oil microcapsules.

Salmon is a typical regressive fish that grows in the sea and returns to fresh water in the spawning season. The oil extracted from salmon and salmon contains a large amount of polyunsaturated fatty acids such as EPA (Eicosapentaenoic acid) and DHA (Docosa hexaenoic acid) Can be usefully used.

However, these polyunsaturated fatty acids extracted from salmon are easily oxidized and decomposed, resulting in generation of unpleasant odors due to the production of lower carbonyl compounds, as well as a detrimental effect on quality such as lowered nutritional value. In order to solve such problems, microencapsulation of oil has been attempted extensively, and microencapsulation of oil having a diameter of several tens of micrometers is typical.

Microencapsulation is a technique for coating the exterior of oil using solid, liquid, or gaseous materials under certain conditions. Owing to the coating, it is possible to protect the oil itself from the external environment such as light, oxygen and moisture and further to block the toxicity and odor, and solidify the fluid having fluidity, Various functions can be given depending on the type.

However, in order to realize such a function through microencapsulation, the coating material used in the microcapsule is basically required to have excellent film-forming ability, excellent solubility, and a precondition that it should not be dissolved or reacted with the nuclear material do. For this reason, microencapsulation of various types of oils extracted from fish has been attempted. However, there has not yet been proposed a microencapsulation method for salmon oil.

Korean Patent No. 0998656, Korean Patent No. 1048271

It is an object of the present invention to provide a microencapsulation method of salmon oil which can secure the stability of food at the same time while improving the industrial utilization of salmon oil and a salmon oil To provide a microcapsule.

In order to accomplish this object, the present invention provides a method of fishing a salmon, comprising: separating a fish frame of a salmon; Drying and crushing the separated fish frame; Extracting salmon oil from a crushed fish frame using a heating method selected from the group consisting of hot water extraction and organic solvent extraction, or a non-heating method such as supercritical extraction or compression extraction; Spray drying the extracted salmon oil to microencapsulate; And the present invention is characterized in that it includes the technical features.

According to the present invention, when salmon oil is extracted and then pulverized, it is possible not only to lower the fat acidity and maintain proper quality even when stored for a long time, but also to enhance the industrial utilization of salmon oil, This is expected to be advantageous.

Figure 1 is a yield comparison chart according to the various methods of salmon oil extraction according to the present invention.
Figure 2 is a fatty acid comparison chart according to various methods of salmon oil extraction according to the present invention.
FIG. 3 is an astaxanthin analysis table of salmon oil extracted by the non-heating method according to the present invention.
Figure 4 is a comparison of the powder yield of salmon oil for various coating materials used in accordance with the present invention.
FIG. 5 is a scanning electron micrograph of microcapsules using coating materials of Maltodextrin, sodium caseinate and WPI in the present invention. FIG.
FIG. 6 is a graph showing changes in pH of the microcapsules using the coating materials of maltodextrin, sodium caseinate and WPI according to the storage period according to the present invention. FIG.
FIG. 7 is a graph of AV change according to storage time of microcapsules using coating materials of Maltodextrin, sodium caseinate and WPI in the present invention. FIG.
8 is a chart of POV changes according to storage time of microcapsules using coating materials of Maltodextrin, sodium caseinate and WPI in the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the technical features of the present invention, A detailed description thereof will be omitted.

The present invention basically comprises a step of separating a fish frame of salmon, a step of drying and crushing a fish frame, a step of extracting salmon oil, and a step of microencapsulating by spray drying. Each of these steps will be described in detail below.

First, remove the fish frame from the salmon. The fish frame, which is called the core bone, is a part of the fish that is separated from the fillet and has some muscles attached to it. It is a healthy functional ingredient such as collagen, calcium and phosphorus, And myofibrillar proteins.

Once the salmon fish frame is detached, it is dried and crushed to a size or less. The drying may be carried out by any of natural drying and heat drying methods. Considering productivity, the thermal drying method may be preferable. The crushing is to increase the surface area to facilitate extraction of the oil. The extent to which it is crushed can vary widely depending on the extraction method.

Once the dried salmon has been crushed into the fish frame, salmon oil is extracted. Extraction of the salmon oil may be by either a heating method or a non-heating method.

The heating method may include hot water extraction and organic solvent extraction. The former method can be performed by extracting oil from a water bath in a state in which a fish frame of crushed salmon is mixed with distilled water and then concentrating it using an evaporator. The latter method can be performed by using an organic solvent using ethanol, methanol, or a nucleic acid solution, extracting the fish frame of crushed salmon with a constant temperature water tank in the state of being mixed with any one of the organic solvents, and concentrating it as an evaporator.

The non-heating method may be supercritical extraction or compression extraction. The former is supercritical carbon dioxide, and supercritical carbon dioxide is injected into a fish frame of a salmon which is crushed to a certain size and filled into an extractor, and then the oil is adsorbed from the fish frame. Separation of supercritical carbon dioxide and salmon oil ≪ / RTI > The latter is a method of extracting salmon oil by squeezing the fish frame of crushed salmon as a compactor.

Once the salmon oil is extracted, the coating material is spray dried into salmon oil followed by microencapsulation. Capsule material can be composed of mixed solution of maltodextrin, chclodextrin, sodium caseinate, gum arabic, whey protein isolate and decaglycerine monooleate as an emulsifier. Once the capsule material is prepared, it is homogenized by mixing with the extracted salmon oil, followed by microencapsulation of the salmon oil using a conventional spray dryer to complete the present invention.

Hereinafter, specific embodiments of the present invention will be described with reference to the accompanying drawings. The oil extraction used fish frame of salmon left after processing step.

Extract of salmon oil

In the hot water extraction, 100 g of the fish frame of crushed salmon and 400 g of distilled water were put into a round flask, and the mixture was extracted in a constant temperature water bath at 100 ° C. for 6 hours and then concentrated using an evaporator. In the organic solvent extraction using ethanol, methanol and nucleic acid solution, 100 g of the fish frame of crushed salmon and 400 g of the solvent were put into a round flask, and the mixture was extracted in a constant temperature water bath at 60 ° C. for 6 hours, concentrated using an evaporator, .

The supercritical extraction was carried out by pressurizing the liquefied carbon dioxide produced by cooling the compressed carbon dioxide to a pressure of 80-700 bar and then heating it to a temperature of 35-90 ° C. In the supercritical fluid extraction step, The supercritical carbon dioxide extraction step was performed by injecting supercritical carbon dioxide 20-30 g / min into the extractor containing the fish frame. Compression extraction was performed by applying a pressure of about 30 MPa to 80 MPa to the fish frame of crushed salmon.

Comparison of yield by each extraction method

The yields of salmon oil according to each extraction method were analyzed by calculating the fish frame content and the extracted oil content of crushed salmon. The results are shown in FIG. As shown in FIG. 1, the yield of hydrothermal extraction was the lowest (12.49%) and ethanol, methanol, and nucleic acids were 29.14%, 19.27 and 44.45%, respectively. The yield of nucleic acid was 44.45% . Supercritical extraction using non - heat extraction method was 44.87% and compression extraction was 43.25%. Supercritical extraction showed the highest yield, but squeezed extraction showed similar values.

Comparison of fatty acids according to each extraction method

Fatty acid analysis of salmon oil was done by extracting lipid with chloroform and methanol by Folch et al. Methylation was carried out in a screw-capped test tube with 80 mg of lipid extracted with Folch method and 0.4 mg of tricosanoic acid methyl esters (0.4 mg / ml hexane, internal standard), and the solvent was removed under a nitrogen purge. Then, 0.5 N NaOH (in methanol) Was added and hydrolyzed at 90 ° C for 7 minutes and then cooled at room temperature for 5 minutes.

Then 1 mL of 14% boron trifluoride (in methanol) was added and methylated at 90 ° C for 10 minutes. The reaction mixture was cooled at room temperature for 30 minutes. 3 mL of hexane and 8 mL of distilled water were added and 1 mL of the upper layer was recovered by GC analysis. The results are shown in FIG. 2. As can be seen from the figure, the fatty acids of the oils according to the respective extraction methods showed no significant difference.

Non-heated  Of salmon oil extracted by methods astaxanthin  analysis

Astaxanthin analysis of supercritical and squeezed salmon oil was used to modify the method of Pavasant et al. The filtrate was filtered through a 0.45 μm membrane filter (Tyko Roshi Kaisha, Japan) and analyzed by HPLC (HITACHI 2000, Tokyo, Japan). HPLC analysis conditions were C18 column (250 × 4.6 mm 5 μm, Waters) and acetonitirile: dichloromethane: ethanol (5:10:85) were used as the solvent. The flow rate was 1.0 mL / min, and the sample injection amount was 10 μL. The astaxanthin standard calibration curves were astaxanthin (Dr. Ehrenstorfer GmbH Co., Germany). The results of the analysis of astaxanthin are shown in Fig. 3. The astaxanthin and salmon oil extracted from supercritical salmon oil were 2.28 mg / 100 g and 3.00 mg / 100 g, respectively.

Spray drying of salmon oil

The salmon oil microencapsulation method of the present invention comprises 10 to 30% by weight of a mixture of maltodextrin, chclodextrin, sodium caseinate, gum arabic and whey protein isolate as a capsule material and 1 to 5% by weight of decaglycerine monooleate as an emulsifier And homogenized at 10,000 rpm for a minute to prepare a coating material mixture. Then, 5 to 30% by weight of extracted salmon oil was mixed and homogenized with homogeniger, and microcapsules of salmon were prepared using a spray drier.

Powder yield of salmon oil with various coating materials

The microencapsulation yield was measured according to the Gallardo et al. Method to determine the microencapsulation yield according to the coating material and blend ratio. That is, the total oil (TO) content in the microcapsules was measured by acid decomposition and solvent extraction method. Transfer 1 g of the microcapsules to a crude fat extraction container, add 10 mL HCl (4 + 1) slowly, boil in a water-bath set at 70 ° C to 100 ° C and boil for 30 minutes.

After the reaction was completed, the reaction mixture was cooled at room temperature, added with 25 mL of ethyl ether and petroleum ether, and shaken vigorously for 1 minute. Then, the mixture was allowed to stand for a predetermined time to separate the supernatant. The solution was collected and filtered (Whatman No. 1). The filtrate was concentrated under reduced pressure, dried under vacuum, and the measured value was expressed as a TO value.

Extractable oil (EO) content, which is not microencapsulated, was measured by organic solvent extraction method. That is, 75 g of ethyl ether was added to 4 g of the microcapsule powder, and the mixture was extracted at 25 ° C. for 15 minutes. After filtration, the filtrate was collected by repeating the above procedure twice more. The collected filtrate was concentrated under reduced pressure, dried under vacuum, and measured for weight. The measured EO value was used to calculate the microencapsulation efficiency. The results are shown in FIG.

The total fat content of the microencapsulated powder after acid decomposition and the content of encapsulated fat after microencapsulation were expressed as the yield (%). The microencapsulation yield of maltodextrin and sodium caseinate was 81.73% and the microencapsulation yield of maltodextrin, sodium caseinate and WPI was 82.55%.

15 times Of the treatment (MD / SC / WPI) SEM

Scanning electron microscopy was used to observe the surface morphology of the microcapsules prepared with MD / SC / WPI (82.55%), which showed the highest yield. As can be seen from Fig. 5, the distribution of the particles was uniform, the texture of the fiber surface appeared smooth, and all the shapes were close to the circular shape. Further, it can be seen that the stability of the capsule is very good considering that the particles do not aggregate or combine with each other.

15 times Treatment MD / SC / WPI's  Storage stability

Microcapsule powder prepared by using MD / SC / WPI as coating material was stored at room temperature (25 ℃) for 30 days and its quality characteristics were analyzed. Quality characteristics were measured for pH, AV (acid value) and POV (peroxide value), respectively.

First, 3 g of the crushed sample was homogenized with a polytron homogenizer (IKA labortechnik T25-B, Malaysia) together with 27 ml of distilled water for 1 minute at 14,000 rpm and measured with a pH meter (Mettler Toledo Co, MP 230, Swiss). As a result, as shown in FIG. 6, the salmon oil powder did not show any significant difference ( p > 0.05) as 5.99 - 6.11 for 30 days of storage.

AV was prepared by dissolving 2 g of crushed sample in a 250 ml Erlenmeyer flask and adding 100 ml of a 2: 1 solution of ether-ethanol as a neutral solvent. To this was added 2-3 drops of the indicator of 1% phenolphthalein solution, titrated with 0.1N KOH-ethanol standard solution, and titrated to the end point when it turned red. As a result, as shown in FIG. 7, the acid value change of the salmon oil powder over the storage period did not show a significant difference and was very stable ( p > 0.05).

POV is prepared by dissolving 2 g of the crushed sample in a 250 ml Erlenmeyer flask, adding 50 ml of chloroform-acetic acid solution, adding 1 ml of KI saturated solution, shaking for 1 minute, allowing to stand for 5 minutes in cool dark place, And mixed by shaking. 1 ml of 1% starch solution was added as an indicator, and 0.01 N Na 2 S 2 O 3 When the solution became colorless, it was titrated to the end point.

As can be seen from FIG. 8, AOV values were significantly increased with storage period ( p <0.05). AOV is related to the early stage of rancidity of lipid oxidation and is a useful index for comparing the rate of oxidation. In the case of the present invention, the quality is maintained properly as 20.64 meq / kg is stored at 30 days of storage ( p < 0.05).

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. It will be apparent that the present invention can be practiced with added features.

Claims (2)

Separating the fish frame of the salmon;
Drying and crushing the separated fish frame;
Extracting salmon oil from a crushed fish frame using a heating method selected from the group consisting of hot water extraction and organic solvent extraction, or a non-heating method such as supercritical extraction or compression extraction;
Spray drying the extracted salmon oil to microencapsulate;
Lt; RTI ID = 0.0 &gt; encapsulation &lt; / RTI &gt;
A salmon oil microcapsule prepared according to claim 1.
KR1020150176727A 2015-12-11 2015-12-11 Quality characterization of salmon oil microencapsulated with various wall materials KR20170069483A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20220155497A (en) 2021-05-14 2022-11-23 허미진 rTG Omega-3 Manufacturing Method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20220155497A (en) 2021-05-14 2022-11-23 허미진 rTG Omega-3 Manufacturing Method

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