CN102925284A - Technique for extracting low-cholesterol-content krill oil from Antarctic krill - Google Patents

Technique for extracting low-cholesterol-content krill oil from Antarctic krill Download PDF

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CN102925284A
CN102925284A CN2012104129794A CN201210412979A CN102925284A CN 102925284 A CN102925284 A CN 102925284A CN 2012104129794 A CN2012104129794 A CN 2012104129794A CN 201210412979 A CN201210412979 A CN 201210412979A CN 102925284 A CN102925284 A CN 102925284A
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krill
shrimp
shrimp sauce
cholesterol
krill oil
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CN102925284B (en
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刘代成
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Shandong Normal University
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Shandong Normal University
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Abstract

The invention discloses a technique for extracting low-cholesterol-content krill oil from Antarctic krill, which comprises the following steps: (1) adding dry Antarctic krill into acetone, and extracting the dry Antarctic krill three times, 1 hour each time; merging the extracting solutions, and carrying rotary evaporation to remove acetone, thereby obtaining krill oil; (2) adding n-hexane into krill slag obtained by filtering after the last extraction in the step (1), and extracting three times, 1 hour each time; merging the extracting solutions, and carrying rotary evaporation to remove the n-hexane, thereby obtaining krill oil; and (3) merging the krill oil in the step (1) and step (2), adding ethanol, stirring to dissolve the krill oil, standing in a freezing environment to naturally stratify the mixed solution, pouring out the upper stratum to obtain a supernatant, and carrying out rotary evaporation to obtain the low-cholesterol-content krill oil. The invention optimizes the Antarctic krill oil extraction technique, so that the cholesterol content in the krill oil is low (0.37-0.51% or so); and the invention enhances the quality of the krill oil, and makes contribution to the development of related Antarctic krill oil products.

Description

A kind of technique of from krill, extracting the shrimp sauce of lower cholesterol content
Technical field
The present invention relates to a kind of technique of from krill, extracting the shrimp sauce of lower cholesterol content.
Background technology
Cholesterol is the cell constituent of the film, is the precursor of steroid hormone in the body, vitamins D and cholic acid, is the good tensio-active agent of pharmaceutical preparation, also is the important component of natural Calculus Bovis and artificial Calculus Bovis, has important pharmaceutical use.Cholesterol is because be the synthetic raw material of hormones, and is expensive, and per kilogram is more than 600 yuan, and can export goods and earn foreign currency in a large number.Cholesterol adds toothpaste, and effect lubricated, that brighten, stop blooding is arranged, and cholesterol also is usually used in the makeup.Cholesterol is because of water insoluble, the adhesion vessel wall that in blood, avales, and artery-clogging causes the various diseases such as heart trouble, the cerebrovascular, and therefore, cholesterol is in higher level in human body be disadvantageous to human body.
The krill aboundresources, at present, countries in the world are less to utilizing of krill, mainly are to be processed into the krill shrimp sauce, have then as bait or feed, Japan then adds it as cooking.The method of existing extraction krill shrimp sauce generally is with hydrophobic solvent such as the extractions such as normal hexane, sherwood oil, contain more cholesterol in the shrimp sauce that its extraction obtains, how reducing the content of cholesterol in the shrimp sauce, the quality of raising shrimp sauce, is current urgent problem.
Summary of the invention
For above-mentioned prior art, the invention provides a kind of technique of from krill, extracting the shrimp sauce of lower cholesterol content, extract the shrimp sauce that obtains through this technique, cholesterol level is low, and the shrimp sauce quality is high.
The present invention is achieved by the following technical solutions:
A kind of technique of from krill, extracting the shrimp sauce of lower cholesterol content, step is as follows:
(1) get the dried krill of 100g (Han Shui Liang Approximately is 8%~10%) and join in 500~600ml acetone, 20~35 ℃ lower extracts dried krill 3 times, extracts 1h at every turn, every extraction once, filtration leaches dried krill; United extraction liquid, at 45~55 ℃, rotary evaporation is removed acetone and is got shrimp sauce (about 6~6.26g) under-0.07~0.09Mpa;
(2) step (1) is last filters to get the shrimp slag after extracting, and adds the normal hexane of 500~600ml in the shrimp slag, and 20~35 ℃ of lower extractions 3 times are extracted 1h at every turn, and every extraction is once filtered the shrimp slag is leached; United extraction liquid, at 45~60 ℃ ,-0.07~-0.09Mpa under rotary evaporation remove normal hexane and get shrimp sauce (about 4.519~4.832g);
(3) combining step (1) and step (2) gained shrimp sauce (cholesterol level is about 3.6%~4.1%), 5~11 times the 80~95%(volume fraction that adds the shrimp sauce quality) ethanol, stirring makes its dissolving, freeze under-20 ℃~-26 ℃ and put 8~14h, the mixed solution natural layering, the upper strata is the ethanolic soln that contains the part shrimp sauce, lower floor is the ethanolic soln (can be used as the raw material that extracts cholesterol) that contains cholesterol and part, pour out the upper strata and get supernatant liquor, supernatant liquor is at 55 ℃~65 ℃, rotate the evaporative removal etoh solvent under-0.07~0.09Mpa, namely get the shrimp sauce of lower cholesterol content, its cholesterol level is about 0.37%~0.51%(massfraction).
The present invention has optimized the technique of extracting the krill shrimp sauce, and cholesterol level is low in the resulting shrimp sauce, is about 0.37%~0.51%, has improved the quality of shrimp sauce, has made contribution for developing relevant krill shrimp sauce product.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1 extracts shrimp sauce from krill
Step is:
(1) dried krill 100g adds acetone 600ml, and 25 ℃ of lower extractions 3 times are extracted 1h at every turn, every extraction once, filtration leaches dried krill; Merge three times extracting solution (about 1500ml), 55 ℃ ,-0.09Mpa under rotation evaporative removal acetone get shrimp sauce 6.26g;
(2) filter to get shrimp slag (83g) after the above-mentioned last extraction, add normal hexane 500ml in the shrimp slag, 25 ℃ of lower extractions 3 times are extracted 1h at every turn, every extraction once, filtration leaches dried krill; Merge three times extracting solution (about 1300ml), at 45 ℃, rotary evaporation is removed normal hexane under the-0.09Mpa, gets shrimp sauce 4.519g;
(3) shrimp sauce of above-mentioned acetone extraction and the shrimp sauce of normal hexane extraction are merged, get shrimp sauce 10.779g, cholesterol level is 3.6% in the shrimp sauce, adds 55ml 80% ethanol in shrimp sauce, stirring makes its dissolving, freeze and be placed on-20 ℃ spend the night (12h), the mixed solution natural layering is poured out the upper strata and is got supernatant liquor, supernatant liquor is at 65 ℃, rotation evaporative removal etoh solvent gets shrimp sauce 8.2g under the-0.09Mpa, and cholesterol level is 0.37% in the survey shrimp sauce.
Cholesterol level detects the following method that adopts in the shrimp sauce:
A ferric ammonium sulfate developer: dissolving 4.463g ferric ammonium sulfate [FeNH 4(SO 4) 212H 2O] in 100ml 85% phosphoric acid, therefrom get the dense H of 80ml 2SO 4Be diluted to 100ml.
The B Specification Curve of Increasing: accurately take by weighing 100mg cholesterol standard substance, be dissolved in the Glacial acetic acid, be diluted to 100ml, namely cholesterol 1mg/ml(is as stock solution); Therefrom get 10ml, be diluted to 100ml with Glacial acetic acid, be i.e. 100 μ g cholesterol/ml standard solutions;
Draw cholesterol standard solution 0.0,0.4,0.8,1.0,1.2ml, place 25ml band plug colorimetric cylinder; In each pipe, add Glacial acetic acid, make cumulative volume reach 4ml, add again 2ml ferric ammonium sulfate developer, shake up immediately, in 30~60min, measure optical density(OD), drawing standard curve in spectrophotometer 560nm wavelength place.
The C sample determination: take by weighing detected sample 100mg, add sherwood oil 5ml dissolving, then petroleum ether solution is moved in another dry test-tube, logical nitrogen dries up in 65 ℃ of water-baths; Add 4ml Glacial acetic acid dissolved residue, add 2ml ferric ammonium sulfate developer, mixing, behind the 30min in the place's colorimetric estimation of spectrophotometer 560nm wavelength, by recording optical density(OD), check in corresponding cholesterol level from typical curve, and then calculate the content of cholesterol in the unit sample.
Embodiment 2 extracts shrimp sauce from krill
Step is:
(1) dried krill 100g adds acetone 550ml, and 35 ℃ of lower extractions 3 times are extracted 1h at every turn, every extraction once, filtration leaches dried krill; Merge three times extracting solution (about 1350ml), 45 ℃ ,-0.07Mpa under rotation evaporative removal acetone get shrimp sauce 6.10g;
(2) filter to get shrimp slag (85g) after the above-mentioned last extraction, add normal hexane 550ml in the shrimp slag, 35 ℃ of lower extractions 3 times are extracted 1h at every turn, every extraction once, filtration leaches dried krill; Merge three times extracting solution (about 1360ml), at 60 ℃, rotary evaporation is removed normal hexane under the-0.07Mpa, gets shrimp sauce 4.610g;
(3) shrimp sauce of above-mentioned acetone extraction and the shrimp sauce of normal hexane extraction are merged, get shrimp sauce 10.71g, cholesterol level is 4.1% in the shrimp sauce, adds 110ml 95% ethanol in shrimp sauce, stirring makes its dissolving, freeze and be placed on-26 ℃ spend the night (12h), the mixed solution natural layering is poured out the upper strata and is got supernatant liquor, supernatant liquor is at 55 ℃, rotation evaporative removal etoh solvent gets shrimp sauce 7.9g under the-0.07Mpa, and cholesterol level is 0.51% in the survey shrimp sauce.
Embodiment 3 extracts shrimp sauce from krill
Step is:
(1) dried krill 100g adds acetone 500ml, and 20 ℃ of lower extractions 3 times are extracted 1h at every turn, every extraction once, filtration leaches dried krill; Merge three times extracting solution (about 1300ml), 55 ℃ ,-0.08Mpa under rotation evaporative removal acetone get shrimp sauce 6g;
(2) filter to get shrimp slag (84g) after the above-mentioned last extraction, add normal hexane 600ml in the shrimp slag, 20 ℃ of lower extractions 3 times are extracted 1h at every turn, every extraction once, filtration leaches dried krill; Merge three times extracting solution (about 1500ml), at 55 ℃, rotary evaporation is removed normal hexane under the-0.08Mpa, gets shrimp sauce 4.832g;
(3) shrimp sauce of above-mentioned acetone extraction and the shrimp sauce of normal hexane extraction are merged, get shrimp sauce 10.832g, cholesterol level is 3.8% in the shrimp sauce, adds 80ml 90% ethanol in shrimp sauce, stirring makes its dissolving, freeze and be placed on-23 ℃ spend the night (12h), the mixed solution natural layering is poured out the upper strata and is got supernatant liquor, supernatant liquor is at 60 ℃, rotation evaporative removal etoh solvent gets shrimp sauce 8.1g under the-0.08Mpa, and cholesterol level is 0.45% in the survey shrimp sauce.

Claims (1)

1. technique of from krill, extracting the shrimp sauce of lower cholesterol content, it is characterized in that: step is as follows:
(1) get the dried krill of 100g and join in 500~600ml acetone, 20~35 ℃ lower extracts dried krill 3 times, extracts 1h at every turn, every extraction once, filtration leaches dried krill; United extraction liquid, at 45~55 ℃, rotary evaporation is removed acetone and is got shrimp sauce under-0.07~0.09Mpa;
(2) step (1) is last filters to get the shrimp slag after extracting, and adds the normal hexane of 500~600ml in the shrimp slag, and 20~35 ℃ of lower extractions 3 times are extracted 1h at every turn, and every extraction is once filtered the shrimp slag is leached; United extraction liquid, at 45~60 ℃ ,-0.07~-0.09Mpa under rotary evaporation remove normal hexane and get shrimp sauce;
(3) combining step (1) and step (2) gained shrimp sauce, 5~11 times 80~95% ethanol that add the shrimp sauce quality, stirring makes its dissolving, freeze under-20 ℃~-26 ℃ and put 8~14h, the mixed solution natural layering is poured out the upper strata and is got supernatant liquor, and supernatant liquor is at 55 ℃~65 ℃, rotate the evaporative removal etoh solvent under-0.07~0.09Mpa, namely get the shrimp sauce of lower cholesterol content.
CN201210412979.4A 2012-10-25 2012-10-25 Technique for extracting low-cholesterol-content krill oil from Antarctic krill Expired - Fee Related CN102925284B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN107384585A (en) * 2017-09-21 2017-11-24 江南大学 A kind of grading system for antarctic krill oil method
CN107903997A (en) * 2017-12-21 2018-04-13 山东师范大学 A kind of method for preparing grease again using the dry shrimp slag of krill degreasing as raw material
CN107904009A (en) * 2017-12-21 2018-04-13 山东师范大学 A kind of method for extracting grease again from krill shrimp slag
CN107964453A (en) * 2017-12-21 2018-04-27 山东师范大学 The method for preparing grease again from the dry shrimp slag of krill degreasing
CN109207247A (en) * 2018-09-25 2019-01-15 深圳先进技术研究院 The preparation method of antarctic krill oil, deodorant antarctic krill oil and its application, food

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CN102643306A (en) * 2012-04-01 2012-08-22 浙江大学 Method for extracting lecithin, egg yolk oil and cholesterol from egg yolk

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CN102041166A (en) * 2011-01-20 2011-05-04 山东师范大学 Method for extracting krill oil with high phosphatide content from Antarctic krills
CN102643306A (en) * 2012-04-01 2012-08-22 浙江大学 Method for extracting lecithin, egg yolk oil and cholesterol from egg yolk

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107384585A (en) * 2017-09-21 2017-11-24 江南大学 A kind of grading system for antarctic krill oil method
CN107903997A (en) * 2017-12-21 2018-04-13 山东师范大学 A kind of method for preparing grease again using the dry shrimp slag of krill degreasing as raw material
CN107904009A (en) * 2017-12-21 2018-04-13 山东师范大学 A kind of method for extracting grease again from krill shrimp slag
CN107964453A (en) * 2017-12-21 2018-04-27 山东师范大学 The method for preparing grease again from the dry shrimp slag of krill degreasing
CN107964453B (en) * 2017-12-21 2021-01-08 山东师范大学 Method for preparing grease from degreased dried euphausia superba residues
CN109207247A (en) * 2018-09-25 2019-01-15 深圳先进技术研究院 The preparation method of antarctic krill oil, deodorant antarctic krill oil and its application, food

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