CN103342669A - Simple method for extracting natural taurine - Google Patents
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Abstract
The invention provides a simple method for extracting natural taurine. The invention is characterized by comprising the following steps: raw material pretreatment: after cleaning seashells, boiling at high temperature, collecting the soup, and concentrating; impurity removal with ethanol: adding ethanol into the concentrated soup to obtain a precipitate and a supernatant; concentrating the supernatant to obtain a concentrated solution; crystallization: adding 3-4 times by volume of anhydrous ethanol into the concentrated solution, immediately carrying out vacuum filtration for impurity removal, standing the filtrate at 4 DEG C to crystallize for more than 24 hours, carrying out vacuum filtration, and drying the solid to obtain the taurine coarse crystal; and for enhancing the purity of the taurine, carrying out recrystallization one or more times as required. The method provided by the invention can effectively utilize seashell processing byproducts and enhance the utilization ratio of ocean resources. The invention has the advantages of simple technique, low extraction cost, high extraction rate, energy saving and environmental protection. The ethanol used in the method can be recycled, thereby being beneficial to industrialized production.
Description
Technical field
The present invention relates to the marine prods manufacture field, more specifically relate to a kind of extract natural taurine soup juice obtained from the shellfish boiling method.
Background technology
Taurine is a kind of nonprotein sulfur amino acid, and chemistry 2 ﹣ taurines by name, be the necessary nutrient substance of human body.Research shows, taurine has increases that cell is anti-oxidant, the ability of Green Tea Extract damage and antiviral infringement.It is good liver-protecting preparation, has the eyesight of increasing, promotion brain development, relieving fatigue, reduction cholesterol, anti-inflammatory, analgesic effect, has certain anti-tumor activity simultaneously.Taurine extensively makes an addition to infant and food for the aged.Along with people's living standard improve constantly and to the understanding gradually of taurine function, the market potential that taurine is produced is huge, economic benefit is very considerable.
At present, the production method of taurine mainly contains synthetic method and biological extraction method.The problems such as the synthetic method has that material toxicity is large, complex operation, investment of production equipment are high, environmental pollution.Utilize the marine prods processing byproduct to extract taurine, raw material sources safety not only, also can improve the utilization ratio of oceanic resources, environmental contamination reduction.But, due to production technique, on world market, the taurine price of natural extract is far above synthetic at present, therefore, the process for preparing natural taurine of setting up high-efficient simple will have huge social benefit and good economic benefit.
At present, domestic most employing ion exchange method is extracted natural taurine.This technique needs large-scale equipment, and cost is higher.And a large amount of bronsted lowry acids and bases bronsted lowry of ion exchange resin regeneration needs, large to the pollution of environment.Therefore, be badly in need of to explore a kind of simple and easy, cost is low, the extracting method of energy-conserving and environment-protective.
According to China Fisheries yearbook statistic data, within 2011, national shellfish output is approximately 1,180 ten thousand tons.At present, the working method of shellfish be mainly after drying after freezing after freezing processing, boiling, boiling, boiling, pickle, tank system etc. after boiling, can produce a large amount of soup juice in the course of processing.These soup juice are except being used on a small quantity produce food flavouring, and major part is used as discharge of wastewater.And in soup juice taurine and free aminoacid content very high, be badly in need of that exploitation is a kind of will discard the method that soup juice uses.
Summary of the invention
The object of the present invention is to provide that a kind of method is simple, cost is low, the taurine extracting method of utilization of waste material, energy-conserving and environment-protective.
For achieving the above object, the invention provides a kind of method of extracting natural taurine, it is characterized in that, it comprises the following steps:
Raw materials pretreatment: after shellfish is cleaned up, boiling under high temperature, collecting soup juice, to be concentrated into solid content be for taurine, to prepare after 5 ~ 10%;
The ethanol removal of impurities: be precipitated thing and supernatant liquor to adding ethanol in described condensed soup juice, preferably adding 95 % ethanol to final concentration is 50～80 %(v/v);
Supernatant concentration obtains concentrated solution;
Crystallization: toward adding suction filtration removal of impurities immediately after 3～4 times of volume dehydrated alcohols in described concentrated solution, more than filtrate is placed in 4 ℃ of standing crystallization 24 h, suction filtration is dried and is obtained the taurine coarse crystal.
Method of the present invention can also comprise the step of recrystallization, be specially toward the hot water that adds 2～5 times of weightmeasurement ratios in described taurine coarse crystal, after dissolving, add gac to stir, suction filtration is removed gac, the filtrate obtained adds more than 3～4 times of volume dehydrated alcohols are placed on 4 ℃ of standing crystallization 24 h, and highly purified taurine crystal is dried and obtained to suction filtration; Optional, can repeat once above re-crystallization step.This step can be selected according to the requirement to purity, can a recrystallization, and also can be according to purity requirement recrystallization repeatedly.
Described high temperature steaming temperature is that 80-120 ℃ of cooking time is 20-60 min, preferably 100 ℃ of lower boiling 40 min.
It is for taurine, to prepare after 5 ~ 10% that the soup juice of described raw materials pretreatment is concentrated into solid content.
Described ethanol removal of impurities is 50～80 %(v/v in soup juice, adding ethanol to final concentration) after, room temperature is placed and is stirred 40～120 min in 2～4 days or 70～80 ℃, is precipitated thing and supernatant liquor; Optional, can repeat that throw out is carried out to 2～3 ethanol and remove miscellaneous operation to improve the taurine yield.
The described supernatant liquor of described concentrated employing with normal pressure concentrated or concentrating under reduced pressure method to be concentrated into soluble solid content be 40～60%, in concentration process, the preferential concentrating under reduced pressure method that adopts is concentrated, and Heating temperature remains on 70～80 ℃, and vacuum keep is at-0.1 ~ 0.09 Mpa.
Described shellfish comprises a species of small clam living in fresh water, clam, variegated clam, oyster etc.
The present invention also protects the taurine obtained prepared according to the methods of the invention.
In method of the present invention:
Raw materials pretreatment, obtain and extract required raw material soup juice.
The ethanol removal of impurities, remove protein, salt and a part of polysaccharide.
Crystallization and/or recrystallization, remove other total free aminoacidss, such as glycine, L-glutamic acid, aspartic acid, L-Ala.Also remove remaining polysaccharide.
Solve the problem that the existing raw materials used cost of natural taurine extraction process is high, extraction process needs large-scale equipment, cost is high, the meeting generation is polluted.This extraction process is simple, extraction cost is low, extraction yield is high, energy-conserving and environment-protective.
After adopting technique scheme, can effectively utilize the processing of aquatic products by product, improve the oceanic resources utilization ratio.Technique of the present invention is simple, extraction cost is low, extraction yield is high, environmental protection.
Contain the impurity such as a large amount of protein, strong electrolyte salt and polysaccharide in the soup juice obtained after shellfish boiling of the present invention, after adopting the ethanol removal of impurities, can effectively remove protein, salt and polysaccharide.So the present invention adopts the ethanol removal of impurities.
The most outstanding advantage of the present invention is that technique is simple, does not need complicated equipment investment, only needs very easy equipment; The present invention only need to use ethanol, and ethanol can recycle, and production cost is low, more is conducive to industrialization.Crystallization of the present invention once can obtain the taurine that purity is 73%, and recrystallization once obtains the taurine that purity is 93%.Further increase the number of times of recrystallization, can reach the purity more than 98%.
The discarded soup juice that the present invention be take after shellfish processing, as raw material extracts natural taurine, can greatly reduce production cost, effectively improves the added value of processing of aquatic products by product.
The accompanying drawing explanation
Fig. 1 is the HPLC detection figure of taurine standard substance;
Fig. 2 is the taurine crystal HPLC detection figure that purity is 92.92%
.
Embodiment
Below describe embodiments of the invention in detail, the example of described embodiment is shown in the drawings.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the described technology of the document in this area or condition or carry out according to product description.The unreceipted person of production firm of agents useful for same or instrument, being can be by the conventional products of commercial acquisition.
embodiment 1:the extraction of natural taurine
(1) raw materials pretreatment: after a species of small clam living in fresh water is cleaned up, in 80 ℃ of lower boiling 60 min, collect soup juice, it is 8% rear as the extraction raw material that the heating of soup juice is concentrated into to solid content;
(2) ethanol removal of impurities: get a species of small clam living in fresh water condensed soup juice 150 mL, add 450 mL 95 % ethanol, stir 40 min under 70 ℃, suction filtration obtains filtrate and throw out.Add 100 mL water and 450 mL ethanol in the throw out obtained, 70 ℃ are stirred 40 min, and suction filtration obtains filtrate and throw out.Merge twice filtrate and obtain supernatant liquor;
(3) concentrated: it is 44.5 % that supernatant liquor is concentrated into soluble solid content by the concentrating under reduced pressure method.In the concentrating under reduced pressure process, temperature remains on 70 ~ 80 ℃, and vacuum keep is at-0.1 ~ 0.09 Mpa;
(4) crystallization: toward adding suction filtration removal of impurities immediately after 3 times of volume dehydrated alcohols in concentrated solution, more than filtrate is placed in 4 ℃ of standing crystallization 24 h.Taurine 0.89 g that purity is 73.26 % is dried and obtained to suction filtration.
Purity detects with HPLC: chromatographic column: Discovery C18 moving phase: methyl alcohol-0.05mol/L sodium acetate buffer (pH 5.3) is flow velocity (50:50): 1 mL/min sample size: 20 μ L detect wavelength: 330 nm column temperatures: room temperature.
embodiment 2:the extraction of natural taurine
(1) raw materials pretreatment: by clam told husky with clean after, in 100 ℃ of lower boiling 40 min, collect soup juice, it is 7% rear as the extraction raw material that the heating of soup juice is concentrated into to solid content;
(2) ethanol removal of impurities: get clam condensed soup juice 300 mL, add 900 mL 95 % ethanol, at 70 ℃, stir 120 min, be precipitated thing and filtrate.Filtrate is with obtaining supernatant liquor after activated carbon treatment;
(3) concentrated: it is 48% that supernatant liquor is concentrated into soluble solid content by the concentrating under reduced pressure method.In the concentrating under reduced pressure process, temperature remains on 70 ~ 80 ℃, and vacuum keep is at-0.1 ~ 0.09 Mpa;
(4) crystallization: toward adding suction filtration removal of impurities immediately after 3 times of volume dehydrated alcohols in concentrated solution, more than filtrate is placed in 4 ℃ of standing crystallization 24 h.Taurine 1.25 g that purity is 79.04 % are dried and obtained to suction filtration.
Purity detects with HPLC: chromatographic column: Discovery C18 moving phase: methyl alcohol-0.05mol/L sodium acetate buffer (pH 5.3) is flow velocity (50:50): 1 mL/min sample size: 20 μ L detect wavelength: 330 nm column temperatures: room temperature.
embodiment 3:the extraction of natural taurine
(1) raw materials pretreatment: by variegated clam told husky with clean after, in 120 ℃ of lower boiling 20 min, collect soup juice, it is 8% rear as the extraction raw material that the heating of soup juice is concentrated into to solid content;
(2) ethanol removal of impurities: get variegated clam condensed soup juice 600 mL, add 1800 mL 95 % ethanol, at 70 ℃, stir 40 min, be precipitated thing and supernatant liquor;
(3) concentrated: it is 45.5 % that supernatant liquor is concentrated into soluble solid content by the concentrating under reduced pressure method.In the concentrating under reduced pressure process, temperature remains on 70 ~ 80 ℃, and vacuum keep is at-0.1 ~ 0.09 Mpa;
(4) crystallization: toward adding suction filtration removal of impurities immediately after 3 times of volume dehydrated alcohols in concentrated solution, more than filtrate is placed in 4 ℃ of standing crystallization 24 h.Taurine coarse crystal 1.31 g are dried and obtained to suction filtration;
(5) recrystallization: after the hot water dissolving who adds 5 times (g/mL) 80 ℃ in taurine coarse crystal 1.31 g of drying, add gac to stir, suction filtration is removed gac.The filtrate obtained adds more than 3 times of volume dehydrated alcohols are placed on 4 ℃ of standing crystallization 24 h.Taurine crystal 0.54 g that purity is 92.92% is dried and obtained to suction filtration.
Purity detects with HPLC: chromatographic column: Discovery C18 moving phase: methyl alcohol-0.05mol/L sodium acetate buffer (pH 5.3) is flow velocity (50:50): the 1mL/min sample size: 20 μ L detect wavelength: 330nm column temperature: room temperature.
Fig. 2 is the HPLC detection figure of taurine crystal; Fig. 1 is that the HPLC of taurine standard substance (Sigma company) detects figure.As can be seen from the figure: in Fig. 1, the appearance time of taurine standard substance is 5.796 min, and in Fig. 2, the appearance time of taurine is 5.803 min, and the not assorted peak of Fig. 2, illustrates that the crystal obtained is highly purified taurine.
embodiment 4:the extraction of natural taurine
(1) raw materials pretreatment: after oyster is cleaned up, in 100 ℃ of lower boiling 40 min, collect soup juice, it is 9% rear as the extraction raw material that the heating of soup juice is concentrated into to solid content;
(2) ethanol removal of impurities: get oyster condensed soup juice 1500 mL, add 4.5 L 95 % ethanol, room temperature is placed 3 days, separates and is precipitated thing and supernatant liquor;
(3) concentrated: it is 46 % that supernatant liquor is concentrated into soluble solid content by the concentrating under reduced pressure method.In the concentrating under reduced pressure process, temperature remains on 70 ~ 80 ℃, and vacuum keep is at-0.1 ~ 0.09 Mpa;
(4) crystallization: toward adding suction filtration removal of impurities immediately after 3 times of volume dehydrated alcohols in concentrated solution, more than filtrate is placed in 4 ℃ of standing crystallization 24 h.Taurine coarse crystal 16.96 g are dried and obtained to suction filtration;
(5) recrystallization: the hot water toward adding 3 times (g/mL) 80 ℃ in taurine coarse crystal 16.96 g of drying, after dissolving, add gac to stir, suction filtration is removed gac.The filtrate obtained adds more than 3 times of volume dehydrated alcohols are placed on 4 ℃ of standing crystallization 24 h.Taurine crystal 6.43 g that purity is 90.46% are dried and obtained to suction filtration.
Repeated recrystallization step twice, taurine crystal 1.93 g that to obtain purity be 98.3%.
Purity detects with HPLC: chromatographic column: Discovery C18 moving phase: methyl alcohol-0.05mol/L sodium acetate buffer (pH 5.3) is flow velocity (50:50): 1 mL/min sample size: 20 μ L detect wavelength: 330 nm column temperatures: room temperature.
Although the above has illustrated and has described embodiments of the invention, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art is not in the situation that break away from principle of the present invention and aim can be changed above-described embodiment within the scope of the invention, modification, replacement and modification.
Claims (7)
1. a method of extracting natural taurine, is characterized in that, it comprises the following steps:
Raw materials pretreatment: after shellfish is cleaned up, boiling under high temperature, collect soup juice, and it is concentrated into to the solid substance weight content is 5 ~ 10%;
The ethanol removal of impurities: add ethanol to described soup juice and be precipitated thing and supernatant liquor, preferably adding concentration is that above ethanol to the final concentration of 95 % is 50～80 %(v/v);
Supernatant concentration is obtained to concentrated solution;
Crystallization: toward adding suction filtration removal of impurities immediately after 3～4 times of volume dehydrated alcohols in described concentrated solution, more than filtrate is placed in 4 ℃ of standing crystallization 24 h, after suction filtration, solid substance is dried and obtained the taurine coarse crystal.
2. the method for the extraction natural taurine of claim 1, it is characterized in that, the step that also comprises recrystallization, be specially toward the 70-80 ℃ of hot water that adds 2～5 times of weightmeasurement ratios in described taurine coarse crystal, after dissolving, add gac to stir, suction filtration is removed gac, and the filtrate obtained adds more than 3～4 times of volume dehydrated alcohols are placed on 4 ℃ of standing crystallization 24 h, solid substance is dried and obtained highly purified taurine crystal after suction filtration; Optional, can repeat once above re-crystallization step.
3. the method for claim 1 or 2 extraction natural taurine, is characterized in that, described high temperature steaming temperature is 80-120 ℃, and cooking time is 20-60 min, preferably 100 ℃ of lower boiling 40 min.
4. the method for claim 1 or 2 extraction natural taurine, it is characterized in that, described ethanol removal of impurities is 50～80 %(v/v in soup juice, adding ethanol to final concentration) after, room temperature is placed and is stirred 40～120 min in 2～4 days or 70～80 ℃, obtains supernatant liquor and throw out; Optional, can repeat that throw out is carried out to 2～3 ethanol and remove miscellaneous operation to improve the taurine yield.
5. the method for claim 1 or 2 extraction natural taurine; it is characterized in that; the described supernatant liquor of described concentrated employing with normal pressure concentrated or concentrating under reduced pressure method to be concentrated into soluble solid content be 40～60%; in concentration process; Heating temperature remains on 70～80 ℃, and vacuum keep is at-0.1 ~ 0.09 Mpa.
6. the method for claim 1 or 2 extraction natural taurine, is characterized in that, described shellfish comprises a species of small clam living in fresh water, clam, variegated clam, oyster etc.
7. the taurine that the arbitrary described method of claim 1-6 prepares.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570593A (en) * | 2013-10-29 | 2014-02-12 | 张苗 | Method for extracting taurine from oysters |
| CN104447427A (en) * | 2014-12-11 | 2015-03-25 | 山东省科学院生物研究所 | Method for extracting taurine from sea cucumber intestines |
| CN104478765A (en) * | 2014-11-27 | 2015-04-01 | 山东好当家海洋发展股份有限公司 | Method for extracting taurine from poached oyster liquid |
| CN104725284A (en) * | 2015-03-06 | 2015-06-24 | 集美大学 | Novel preparation method for natural taurine |
| CN104788348A (en) * | 2015-04-30 | 2015-07-22 | 邓鑫 | Method for extracting natural taurine from pearl shells |
| CN104829501A (en) * | 2015-03-24 | 2015-08-12 | 辽宁双增生物工程有限公司 | A method of extracting taurine from a mactra chinensis water decoction |
| CN105523966A (en) * | 2015-12-29 | 2016-04-27 | 广西钦州市绿源天然食品加工有限公司 | A method of extracting taurine from scallop skirt |
| CN105842260A (en) * | 2016-03-21 | 2016-08-10 | 集美大学 | Method for identifying natural taurine and synthetic taurine |
| CN106093078A (en) * | 2016-07-22 | 2016-11-09 | 集美大学 | A kind of method differentiating natural taurine and synthesizing taurine |
| CN113135844A (en) * | 2020-01-17 | 2021-07-20 | 大连鑫玉龙海洋生物种业科技股份有限公司 | Method for extracting taurine from sea cucumber intestines |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570593A (en) * | 2013-10-29 | 2014-02-12 | 张苗 | Method for extracting taurine from oysters |
| CN104478765A (en) * | 2014-11-27 | 2015-04-01 | 山东好当家海洋发展股份有限公司 | Method for extracting taurine from poached oyster liquid |
| CN104478765B (en) * | 2014-11-27 | 2016-06-15 | 山东好当家海洋发展股份有限公司 | A kind of oyster water cooking liquid extracts the method for taurine |
| CN104447427A (en) * | 2014-12-11 | 2015-03-25 | 山东省科学院生物研究所 | Method for extracting taurine from sea cucumber intestines |
| CN104725284A (en) * | 2015-03-06 | 2015-06-24 | 集美大学 | Novel preparation method for natural taurine |
| CN104829501A (en) * | 2015-03-24 | 2015-08-12 | 辽宁双增生物工程有限公司 | A method of extracting taurine from a mactra chinensis water decoction |
| CN104788348A (en) * | 2015-04-30 | 2015-07-22 | 邓鑫 | Method for extracting natural taurine from pearl shells |
| CN105523966A (en) * | 2015-12-29 | 2016-04-27 | 广西钦州市绿源天然食品加工有限公司 | A method of extracting taurine from scallop skirt |
| CN105842260A (en) * | 2016-03-21 | 2016-08-10 | 集美大学 | Method for identifying natural taurine and synthetic taurine |
| CN105842260B (en) * | 2016-03-21 | 2019-04-16 | 集美大学 | A kind of discrimination method of natural taurine and synthesizing taurine |
| CN106093078A (en) * | 2016-07-22 | 2016-11-09 | 集美大学 | A kind of method differentiating natural taurine and synthesizing taurine |
| CN113135844A (en) * | 2020-01-17 | 2021-07-20 | 大连鑫玉龙海洋生物种业科技股份有限公司 | Method for extracting taurine from sea cucumber intestines |
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