CN101548782A - Method for extracting fish oil by utilizing mackerel heads or squid viscera - Google Patents
Method for extracting fish oil by utilizing mackerel heads or squid viscera Download PDFInfo
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- CN101548782A CN101548782A CNA2008100605066A CN200810060506A CN101548782A CN 101548782 A CN101548782 A CN 101548782A CN A2008100605066 A CNA2008100605066 A CN A2008100605066A CN 200810060506 A CN200810060506 A CN 200810060506A CN 101548782 A CN101548782 A CN 101548782A
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- 238000000034 method Methods 0.000 title claims abstract description 55
- 210000001835 viscera Anatomy 0.000 title claims abstract description 34
- 241000238366 Cephalopoda Species 0.000 title claims abstract description 32
- 241000269821 Scombridae Species 0.000 title claims abstract description 30
- 235000020640 mackerel Nutrition 0.000 title claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 31
- 238000004108 freeze drying Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 9
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 9
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 9
- 239000012188 paraffin wax Substances 0.000 claims abstract description 9
- 239000000284 extract Substances 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 13
- 241000251468 Actinopterygii Species 0.000 claims description 10
- 235000019688 fish Nutrition 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 4
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 239000012267 brine Substances 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- 238000007710 freezing Methods 0.000 abstract description 10
- 230000008014 freezing Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 238000010298 pulverizing process Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000002002 slurry Substances 0.000 abstract 3
- 239000000470 constituent Substances 0.000 abstract 1
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- 239000000047 product Substances 0.000 description 14
- MBMBGCFOFBJSGT-KUBAVDMBSA-N all-cis-docosa-4,7,10,13,16,19-hexaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 description 11
- 235000020669 docosahexaenoic acid Nutrition 0.000 description 10
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- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
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- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
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- 238000000638 solvent extraction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
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- Fats And Perfumes (AREA)
Abstract
The invention relates to a method for extracting fish oil by utilizing mackerel heads or squid viscera. The method comprises the following steps: pulverizing primarily washed mackerel heads or squid viscera into slurry by a pulverizer; freezing to dry the slurry ground materials and grinding the slurry ground materials by a grinder; using lower paraffin hydrocarbon as a solvent for extracting the treated ground materials; recovering the solvent and preparing course fish oil; using salt water to wash the prepared course fish oil to obtain the fish oil. The method combines a freeze drying technology with the solvent for extracting the fish oil in the mackerel heads or the squid viscera at low temperature, keeps the original activities and structures of organisms and ensures that effective constituents in the fish oil are stable and the fish oil which is not easy to oxidize is obtained.
Description
Technical field
The present invention relates to from the fish processing byproduct, extract the method for fish oil, relate in particular to a kind of method of utilizing mackerel head or squid viscera to extract fish oil.
Background technology
Contain needed by human unrighted acids such as abundant ω-3 series in the fish oil, particularly be eicosapentaenoic acid (Eicosapentaenoic Acid EPA), (Docosahexaenoic Acid DHA), has been widely used in medicine, health products, the food DHA.EPA, DHA content are especially high in ocean fish, and the main effect of deep sea fish oil has: reduce cholesterol, prevention cardiovascular disease; Preclude blood is solidified and thrombosis, relaxes apoplexy; Reduce artery sclerosis and hypertension; Reduce blood viscosity, stimulate circulation; Improve memory, prevent effect such as aging, its effect that prevents the metastasis of cancer just under study for action.
The fishery of China processing at present is also fairly simple, the waste by-product of some fishery processing is not well utilized, the pollution of environment and the waste of resource have been caused, as having adopted simple method to be processed into fish meal fish guts, the first-class inedible part of fish, still this fish meal moisture instability, oxidation easily, value preserving phase lack.Also there is the method for the hair fish processing fish oil that utilizes shark liver, salmon or low value on ground such as China Fujian, and method for processing mainly adopts the method for Steam Heating distillation.This method exists unsurmountable defective, as it is more limited to process the source of used shark, salmon, the way that steam adds thermal distillation can quicken again fish oil oxidation, improve the quality of acid value and iodine value, reduction fish oil.It is reported the technology of utilizing fish guts and fish processing byproduct to make fish oil and fish meal is also arranged, this technology also all adopts the Steam by water bath cooking method mostly, as: Chinese patent Granted publication number is 1293175C, the patent No. is 200410011213, the day for announcing is on January 3rd, 2007, invention and created name is the patent of " wall pollack fish guts oil extracting method ", the method for disclosed extraction for will simple boiling partition method widen freeze analyse, boiling, squeezing three go on foot the one method.Disclose simultaneously " Chinese marine drug " magazine in its specification, 1999,18 (1) once reported and utilize squid viscera self enzyme hydrolysis internal organ and other refuses to develop, and developed the method for Squid Oil.CSTAD achievement project year is numbered 99014345, and Nanjing University of Chemical Technology, Jiangsu Fresh Water Aquatic Product Inst. adopt and add method and the enzymatic isolation method extraction fish guts oil tech that mixes antioxidant.Freezing back uses milling process to make the technology of fish oil, exist the defective that separation rate is low, the acid value of fish oil is high, and enzymatic hydrolysis to extract fish oil be that control protease optimum pH and temperature are hydrolyzed, centrifugation gets fish oil, because process conditions are difficult to control, be not suitable for industrial production.The present invention adopts the solvent extraction grease, the recovery rate height; Adopt boulton process, make grease be difficult for oxidation; Adopt the salt water washing, can be with soluble impurity flush away in the thick oil that extracts.
Summary of the invention
The objective of the invention is to have kept biological original activity and structure, make stable effective ingredients in the fish oil, obtain being difficult for the fish oil of oxidation by using Freeze Drying Technique at low temperatures in conjunction with the fish oil in solvent extraction mackerel head or the squid viscera.Freeze drying be wet stock (or solution) is frozen into solid-state, will be wherein solid state crystallization water directly distil and be the dewatered dry run of gaseous state, also claim lyophilization.The temperature of freezing is-15～-30 ℃, and cryodesiccated temperature is-30～-50 ℃, and vacuum is 40～200Pa.
Concrete steps of the present invention are as follows:
A kind of method of utilizing mackerel head or squid viscera to extract fish oil is characterized in that may further comprise the steps:
A, will be ground into pulpous state with pulverizer through preliminary fish head or the internal organ that cleaned;
B, will freeze earlier, carry out freeze drying again through the crushed material of pulpous state;
C, will pulverize with pulverizer through the freeze drying thing after the b step process;
D, usefulness lower paraffin hydrocarbon extract the crushed material after the c step process as solvent, and the consumption of solvent is 5-20 a times of the crushed material weight after the c step process, and extracting temperature is 0-50 ℃, and extraction time is 0.5-5 hour;
E, usefulness vacuum concentration method reclaim solvent, and thickening temperature is 10-55 ℃, makes crude fish oil;
F, be the above-mentioned crude fish oil that makes of salt water washing of 1-35%, remove the soluble impurity in the degrease with concentration, fish oil.
Described a kind of method of utilizing mackerel head or squid viscera to extract fish oil, the optimum extraction temperature in the steps d is 10 ℃.
Described a kind of method of utilizing mackerel head or squid viscera to extract fish oil, the optimum solvent in the steps d is benzinum or n-hexane.
Described a kind of method of utilizing mackerel head or squid viscera to extract fish oil, the optimum extraction number of times in the steps d is a secondary, the time respectively is 60 minutes.
Described a kind of method of utilizing mackerel head or squid viscera to extract fish oil, the optimum solvent consumption in the steps d are 15 times of crushed material weight after the c step process.
Described a kind of method of utilizing mackerel head or squid viscera to extract fish oil, the optimum vacuum thickening temperature among the step e is 45 ℃.
Described a kind of method of utilizing mackerel head or squid viscera to extract fish oil, the best brine strength among the step f is 5%.
The present invention has kept biological original activity and structure by freeze-drying, makes stable components.In the freezing process before the freeze-drying because the puncture effect of ice crystal, punctured grease-contained cell, make grease easier being extracted in later process, again because baking temperature is low, drying under vacuum condition, make the prepared fish oil of the present invention more stable than the effective ingredient in the fish oil of existing fish oil extracting method acquisition, activity is more arranged, the grease dissolution rate is higher.
The specific embodiment
The invention will be further described below in conjunction with embodiment.But they are not limitation of the invention.
Embodiment 1
1, gets 1000 gram squid visceras, wash with clear water;
2, squid viscera is rubbed pulp with the stainless steel pulverizer;
3, the product with above-mentioned pulverizing freezes then to carry out freeze drying with freeze drier, and the temperature of freezing is controlled at-15～-30 ℃, and cryodesiccated temperature is controlled at-30～-50 ℃, and vacuum degree control is at 40～200Pa;
4, the freeze drying product is pulverized with pulverizer;
5, temperature is controlled at 10 ℃, and the benzinum of 15 times of dry squid viscera crushed material weight after handling through above-mentioned steps is that solvent extracts; Extract at twice, extracted 60 minutes at every turn, merge extracted twice liquid;
6, temperature is controlled at 45 ℃, adopts the vacuum concentration method that the lower paraffin hydrocarbon volatilization is obtained crude fish oil, and vacuum is 10～100Pa, collects solvent simultaneously, and this solvent can reclaim and add utilization again;
7, the above-mentioned thick oil of salt water washing of utilization 5% concentration removes the soluble impurity in the degrease, can obtain to contain fish oil 331 grams of 50%DHA, EPA.
Embodiment 2
1, gets 1000 gram mackerel heads, wash with clear water;
2, the mackerel head is rubbed pulp with the stainless steel pulverizer;
3, the product with above-mentioned pulverizing freezes then to carry out freeze drying with freeze drier, and the temperature of freezing is controlled at-15～-30 ℃, and cryodesiccated temperature is controlled at-30～-50 ℃, and vacuum degree control is at 40～200Pa;
4, the freeze drying product is pulverized with pulverizer;
5, temperature is controlled at 10 ℃, and the n-hexane of 15 times of dry mackerel crushed material weight after handling through above-mentioned steps is that solvent extracts; Extract at twice, extracted 60 minutes at every turn, merge extracted twice liquid;
6, temperature is controlled at 45 ℃, adopts the vacuum concentration method that the lower paraffin hydrocarbon volatilization is obtained crude fish oil, and vacuum is 10～100Pa, collects solvent simultaneously, and this solvent can reclaim and add utilization again;
7, the above-mentioned thick oil of salt water washing of utilization 5% concentration removes the soluble impurity in the degrease, can obtain to contain fish oil 350 grams of 50%DHA, EPA.
Embodiment 3:
1, gets 1000 gram mackerel heads, wash with clear water;
2, the mackerel head is rubbed pulp with the stainless steel pulverizer;
3, the product with above-mentioned pulverizing freezes then to carry out freeze drying with freeze drier, and the temperature of freezing is controlled at-15～-30 ℃, and cryodesiccated temperature is controlled at-30～-50 ℃, and vacuum degree control is at 40～200Pa;
4, the freeze drying product is pulverized with pulverizer;
5, temperature is controlled at 10 ℃, and the benzinum of 15 times of dry mackerel crushed material weight after handling through above-mentioned steps is that solvent extracts; Extract twice, extracted 30 minutes at every turn, merge extracted twice liquid;
6, temperature is controlled at 45 ℃, adopts the vacuum concentration method that the lower paraffin hydrocarbon volatilization is obtained crude fish oil, and vacuum is 10～100Pa, collects solvent simultaneously, and this solvent can reclaim and add utilization again;
7, the above-mentioned thick oil of salt water washing of utilization 1% concentration removes the soluble impurity in the degrease, can obtain to contain fish oil 240 grams of 50%DHA, EPA.
Embodiment 4
1, gets 1000 gram squid visceras, wash with clear water;
2, squid viscera is rubbed pulp with the stainless steel pulverizer;
3, the product with above-mentioned pulverizing freezes then to carry out freeze drying with freeze drier, and the temperature of freezing is controlled at-15～-30 ℃, and cryodesiccated temperature is controlled at-30～-50 ℃, and vacuum degree control is at 40～200Pa;
4, the freeze drying product is pulverized with pulverizer;
5, temperature is controlled at 0 ℃, and the n-hexane of 5 times of dry squid viscera crushed material weight after handling through above-mentioned steps is that solvent extracts; Extracted 2 hours, and got extract;
6, temperature is controlled at 10 ℃, adopts the vacuum concentration method that the lower paraffin hydrocarbon volatilization is obtained crude fish oil, and vacuum is 10～100Pa, collects solvent simultaneously, and this solvent can reclaim and add utilization again;
7, the above-mentioned thick oil of salt water washing of utilization 35% concentration removes the soluble impurity in the degrease, can obtain to contain fish oil 150 grams of 50%DHA, EPA.
Embodiment 5
1, gets 1000 gram squid visceras, wash with clear water;
2, squid viscera is rubbed pulp with the stainless steel pulverizer;
3, the product with above-mentioned pulverizing freezes then to carry out freeze drying with freeze drier, and the temperature of freezing is controlled at-15～-30 ℃, and cryodesiccated temperature is controlled at-30～-50 ℃, and vacuum degree control is at 40～200Pa;
4, the freeze drying product is pulverized with pulverizer;
5, under the control 50 degree temperature, No. six light petrols of 20 times of dry squid viscera crushed material weight after handling through above-mentioned steps are that solvent extracts; Extracted 5 hours, and got extract;
6, under 55 degree, adopt the vacuum concentration method that the lower paraffin hydrocarbon volatilization is obtained crude fish oil, vacuum is 10～100Pa, collects solvent simultaneously, this solvent can reclaim and add utilization again;
7, the above-mentioned thick oil of salt water washing of utilization 1% concentration removes the soluble impurity in the degrease, can obtain to contain fish oil 253 grams of 50%DHA, EPA.
Embodiment 6
1, gets 1000 gram mackerel fish heads, wash with clear water;
2, mackerel fish head is rubbed pulp with the stainless steel pulverizer;
3, the product with above-mentioned pulverizing freezes then to carry out freeze drying with freeze drier, and the temperature of freezing is controlled at-15～-30 ℃, and cryodesiccated temperature is controlled at-30～-50 ℃, and vacuum degree control is at 40～200Pa;
4, the freeze drying product is pulverized with pulverizer;
5, under the control 30 degree temperature, the n-hexane of 10 times of dry mackerel crushed material weight after handling through above-mentioned steps is that solvent extracts; Extracted 30 minutes, and got extract;
6, under 45 degree, adopt the vacuum concentration method that the lower paraffin hydrocarbon volatilization is obtained crude fish oil, vacuum is 10～100Pa, collects solvent simultaneously, this solvent can reclaim and add utilization again;
7, the above-mentioned thick oil of salt water washing of utilization 20% concentration removes the soluble impurity in the degrease, can obtain to contain fish oil 210 grams of 50%DHA, EPA.
Claims (7)
1. method of utilizing mackerel head or squid viscera to extract fish oil is characterized in that may further comprise the steps:
A, will be ground into pulpous state with pulverizer through preliminary fish head or the internal organ that cleaned;
B, will freeze earlier, carry out freeze drying again through the crushed material of pulpous state;
C, will pulverize with pulverizer through the freeze drying thing after the b step process;
D, usefulness lower paraffin hydrocarbon extract the crushed material after the c step process as solvent, and the consumption of solvent is 5-20 a times of the crushed material weight after the c step process, and extracting temperature is 0-50 ℃, and extraction time is 0.5-5 hour;
E, usefulness vacuum concentration method reclaim solvent, and thickening temperature is 10-55 ℃, makes crude fish oil;
F, be the above-mentioned crude fish oil that makes of salt water washing of 1-35%, remove the soluble impurity in the degrease with concentration, fish oil.
2. a kind of method of utilizing mackerel head or squid viscera to extract fish oil according to claim 1 is characterized in that the extraction temperature in the steps d is 10 ℃.
3. a kind of method of utilizing mackerel head or squid viscera to extract fish oil according to claim 1 is characterized in that the solvent in the steps d is benzinum or n-hexane.
4. a kind of method of utilizing mackerel head or squid viscera to extract fish oil according to claim 1 is characterized in that the extraction time in the steps d is divided into secondary, and the time respectively is 60 minutes.
5. a kind of method of utilizing mackerel head or squid viscera to extract fish oil according to claim 1 is characterized in that the solvent load in the steps d is 15 times of the crushed material weight after the c step process.
6. a kind of method of utilizing mackerel head or squid viscera to extract fish oil according to claim 1 is characterized in that the thickening temperature among the step e is 45 ℃.
7. a kind of method of utilizing mackerel head or squid viscera to extract fish oil according to claim 1 is characterized in that the brine strength among the step f is 5%.
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| CNA2008100605066A CN101548782A (en) | 2008-04-01 | 2008-04-01 | Method for extracting fish oil by utilizing mackerel heads or squid viscera |
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| CNA2008100605066A CN101548782A (en) | 2008-04-01 | 2008-04-01 | Method for extracting fish oil by utilizing mackerel heads or squid viscera |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260585A (en) * | 2011-06-28 | 2011-11-30 | 泰祥集团技术开发有限公司 | Method for extracting fish oil from squid viscera by using animal proteolytic enzyme |
| CN103451005A (en) * | 2013-08-23 | 2013-12-18 | 福州海汇生物科技实业有限公司 | Method for extracting squid oil from leftovers of fresh squids |
| CN103584185A (en) * | 2013-10-28 | 2014-02-19 | 西京学院 | Comprehensive utilization method of canned sardine meat wastes |
| CN104479859A (en) * | 2014-11-27 | 2015-04-01 | 威海博宇食品有限公司 | Preparation method of roe extract |
| CN104611128A (en) * | 2015-01-13 | 2015-05-13 | 浙江工业大学 | Fishy smell-removed fish oil and preparation method thereof |
| CN107822142A (en) * | 2017-11-21 | 2018-03-23 | 荣成海锐芯生物科技有限公司 | A kind of method that cod liver oil capsule is prepared from cod internal organ |
| CN117801877A (en) * | 2023-12-04 | 2024-04-02 | 江西师范大学 | Snakehead viscera crude fish oil refining process, characterization method and application thereof |
-
2008
- 2008-04-01 CN CNA2008100605066A patent/CN101548782A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260585A (en) * | 2011-06-28 | 2011-11-30 | 泰祥集团技术开发有限公司 | Method for extracting fish oil from squid viscera by using animal proteolytic enzyme |
| CN103451005A (en) * | 2013-08-23 | 2013-12-18 | 福州海汇生物科技实业有限公司 | Method for extracting squid oil from leftovers of fresh squids |
| CN103584185A (en) * | 2013-10-28 | 2014-02-19 | 西京学院 | Comprehensive utilization method of canned sardine meat wastes |
| CN103584185B (en) * | 2013-10-28 | 2014-12-31 | 西京学院 | Comprehensive utilization method of canned sardine meat wastes |
| CN104479859A (en) * | 2014-11-27 | 2015-04-01 | 威海博宇食品有限公司 | Preparation method of roe extract |
| CN104611128A (en) * | 2015-01-13 | 2015-05-13 | 浙江工业大学 | Fishy smell-removed fish oil and preparation method thereof |
| CN104611128B (en) * | 2015-01-13 | 2017-09-22 | 浙江工业大学 | Fishy smell-removed fish oil and preparation method thereof |
| CN107822142A (en) * | 2017-11-21 | 2018-03-23 | 荣成海锐芯生物科技有限公司 | A kind of method that cod liver oil capsule is prepared from cod internal organ |
| CN117801877A (en) * | 2023-12-04 | 2024-04-02 | 江西师范大学 | Snakehead viscera crude fish oil refining process, characterization method and application thereof |
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