CN103936874A - Method for extracting sea cucumber polysaccharide from sea cucumber boiled juice - Google Patents
Method for extracting sea cucumber polysaccharide from sea cucumber boiled juice Download PDFInfo
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- CN103936874A CN103936874A CN201410114488.0A CN201410114488A CN103936874A CN 103936874 A CN103936874 A CN 103936874A CN 201410114488 A CN201410114488 A CN 201410114488A CN 103936874 A CN103936874 A CN 103936874A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
A disclosed method for extracting sea cucumber polysaccharide from sea cucumber boiled juice is characterized by comprising technological steps of ultramicro filtering, standing precipitation, filtering, ultramicro membrane separation, spray drying, supercritical extraction, vacuum drying, and obtaining of the sea cucumber polysaccharide product. Because the sea cucumber active polysaccharide, which has health-care efficacy of regulating immune, resisting and preventing cancers and the like, is extracted from the sea cucumber boiled juice, the raw material cost is substantially reduced, the discharge amount of a sea cucumber processing waste liquid is reduced, and pollution to environment is reduced.
Description
Technical field:
The present invention relates to Holothurian machining technical field, is a kind of method that boiled sea cucumber juice extracts sea cucumber polysaccharide specifically.
Background technology:
Sea cucumber is a kind of famous and precious precious marine product, is also a kind of health-care tonic good merchantable brand, and research finds in sea cucumber, to have the functional factor of the effect such as immunomodulatory, anti-cancer and cancer-preventing, is mainly the Stichopus japonicus mucopolysaccharide in its body; The content of this active polysaccharide in sea cucumber body is little, taking traditional salt dry Stichopus japonicus as example, approximately only has 3-5 gram of active polysaccharide in one kilogram of salt dry Stichopus japonicus.
At present, the research of sea cucumber polysaccharide is focused mostly in research fields such as its structure, functions.Sea cucumber polysaccharide nourishing function is very high, but because sea cucumber raw material costliness is directly extracted active polysaccharide taking sea cucumber as raw material, cost is very high, and the therefore extraction of sea cucumber polysaccharide, application are restricted.
Holothurian machining process, generally all will first cut fresh sea cucumber, remove open moisture and the internal organ in abdomen, then adds water and boils, and its body wall is further dewatered, so that processing is thereafter with dry.In this process, produce a large amount of boiled sea cucumber juices, this part liquor is not utilized effectively at present, and processing enterprise is the salt solution of the different concns using in itself and following process, together as processing waste water, and directly discharge; And in the waste water of these discharges, contain the nutritive ingredients such as rich in protein, carbohydrate, inorganic salt, serious environment pollution after discharge.
Research and analyse discovery, in this part waste water, not only contain rich in protein, amino acid and some special acids, as taurine etc., but also the sea cucumber active polysaccharide that contains rich content.Analytical results shows, approximately the active polysaccharide content in 19L boiled sea cucumber juice, is equivalent to the content in 1kg salt dry Stichopus japonicus; Further research is found, comparison of ingredients complexity in boiled sea cucumber juice, except containing active polysaccharide, main impurity component is protein, small-molecule peptide, amino acid, saponin and inorganic salt etc., successfully separating of these impurity and active polysaccharide, it is the key that polysaccharide extracts.
Summary of the invention:
The object of the invention is to overcome the deficiency of above-mentioned prior art, and provide a kind of boiled sea cucumber juice to extract the method for sea cucumber polysaccharide; After mainly solving existing boiled sea cucumber juice discharge, cause the problems such as nutritive ingredient waste while serious environment pollution.
Technical scheme of the present invention is: boiled sea cucumber juice extracts the method for sea cucumber polysaccharide, and its special character is, comprises the steps:
A hyperfiltration, selects the hyperfiltration film of molecular weight cut-off 20000-80000, and the boiled sea cucumber juice of collecting is carried out to hyperfiltration, and supplements and add distilled water or pure water wherein;
B staticly settles, and discards the liquid that sees through in ultra-filtration process, collect trapped fluid, and to add wherein concentration is the tanning solution of 18-20%, and addition is the 2-10% of collected trapped fluid volume, mixes, and leaves standstill 5-20 hour;
C filters, and with 100 object filter-cloth filterings, filter residue discards, and collects filtrate;
D ultra micro membrane sepn, selects the hyperfiltration film of molecular weight cut-off 20000-80000, and the filtrate of collecting is carried out to hyperfiltration, and supplements and add distilled water or pure water wherein;
E spraying is dry, discards the liquid that sees through in ultra-filtration process, collects trapped fluid, and sprays dry with Highspeedcentrifugingandsprayingdrier to it;
F supercritical extraction, collects the dry gained dry powder of spraying, extracts degreasing with supercritical carbon dioxide extraction apparatus; The component being extracted with carbonic acid gas, for extracting Sea Cucumber Glycosides research;
G vacuum-drying, the solid ingredient staying in extraction kettle, with the spirituous solution washing of 70-90%, continues to use after the alcohol slops after washing reclaims; Solids component after washing, is placed in vacuum-drying and is dried;
H sea cucumber polysaccharide product, dry rear gained faint yellow solid is the sea cucumber polysaccharide product of extraction, and wherein sea cucumber polysaccharide content is 80-90%.
Further, the spraying described in e step is dry, and condition is: import hot blast temperature 130-180 DEG C, and outlet 60-80 DEG C, the spray velocity of feed liquid is: 5-15L/h.
Further, the extraction degreasing described in f step, condition is: dry powder loading amount 500-1500g, extraction kettle pressure 15-30Mp, extraction kettle temperature room temperature to 40 DEG C, separating still pressure 5-20Mp, separating still temperature room temperature is to 40-60 DEG C, carbon dioxide flow 20-30L/h, extraction time 0.5-2h.
Further, dry described in g step, condition is: temperature 30-50 DEG C, the absolute pressure 100-5000p in dry epoch, time of drying 1-5 hour.
Compared with the prior art the method that boiled sea cucumber juice of the present invention extracts sea cucumber polysaccharide has outstanding substantive distinguishing features and marked improvement, utilize molecular specific precipitation technology, membrane separation technique, spray drying technology and supercritical extraction technique, by separation and Extraction in boiled sea cucumber juice there is the sea cucumber active polysaccharide of the health-care effect such as immunomodulatory, anti-cancer and cancer-preventing, not only greatly reduce raw materials cost, and reduced the discharge of Holothurian machining waste liquid, reduce the pollution to environment.
Embodiment:
For Comprehension and Implementation better, describe the present invention in detail below in conjunction with embodiment; Illustrated embodiment is only for explaining the present invention, not for limiting the scope of the invention.
Embodiment 1, selects the hyperfiltration film of molecular weight cut-off 50000, and the boiled sea cucumber juice of collecting is carried out to hyperfiltration; In the time finding that the filtration velocity of film declines to some extent, supplement and add distilled water (or pure water) wherein, so that it is substantially constant to maintain the filtration velocity of film; In the process of filtering, the ultrafiltrated of often getting outflow drips Silver Nitrate, survey the amount of chlorion wherein, when finding do not have chlorion to flow out, drip after Silver Nitrate and do not precipitate appearance in ultrafiltrated, stop adding distilled water, continue ultrafiltration 10-20 minute, generally in this process, will consume boiled sea cucumber juice volume 3-5 distilled water doubly; Such as, ultrafiltration 100L boiled sea cucumber juice, approximately need to add 300-500L distilled water; Discard in ultra-filtration process seeing through liquid, collect trapped fluid, and to add wherein concentration be 19% tanning solution, addition is 6% of collected trapped fluid volume, mixes, and leaves standstill 12.5 hours; With 100 object filter-cloth filterings, filter residue discards, and collects filtrate; The hyperfiltration film of selecting molecular weight cut-off 80000, carries out hyperfiltration to the filtrate of collecting.In the time finding that the filtration velocity of film declines to some extent, supplement and add distilled water (or pure water) wherein, so that it is substantially constant to maintain the filtration velocity of film.In the process of filtering, the ultrafiltrated of often getting outflow drips ferric ion, survey the amount of tannin wherein, when finding do not have tannin to flow out, dripping after ferric ion does not have colour-change to occur in ultrafiltrated, stop adding distilled water, continue ultrafiltration 10-20 minute, generally in this process, will consume boiled sea cucumber juice volume 1-2 distilled water doubly; Discard in ultra-filtration process seeing through liquid, collect trapped fluid, and it is dry that it spray with Highspeedcentrifugingandsprayingdrier, the drying conditions of spraying is: 170 DEG C of import hot blast temperatures, export 70 DEG C; The spray velocity of feed liquid is: 12L/h; Collect the dry gained dry powder of spraying, extract degreasing with supercritical carbon dioxide extraction apparatus, condition is: dry powder loading amount 1000g, extraction kettle pressure 22.5Mp, extraction kettle temperature room temperature to 50 DEG C; Separating still pressure 12.5Mp, separating still temperature room temperature to 50 DEG C; Carbon dioxide flow 25L/h, extraction time 1.25h; The component being extracted with carbonic acid gas, for extracting Sea Cucumber Glycosides research; The solid ingredient staying in extraction kettle, the spirituous solution repetitive scrubbing with 90% three times, continues to use after the alcohol slops after washing reclaims; Solids component after washing, is placed in Vacuumdrier dry, and drying conditions is: 40 DEG C of temperature, the absolute pressure 2500p in dry epoch, 3 hours time of drying; After dry, gained faint yellow solid is the sea cucumber polysaccharide product of extraction, and wherein sea cucumber polysaccharide content is 80-90%.
Embodiment 2, selects the hyperfiltration film of molecular weight cut-off 20000, and the boiled sea cucumber juice of collecting is carried out to hyperfiltration, and supplements and add distilled water or pure water wherein; Discard the liquid that sees through in ultra-filtration process, collect trapped fluid, and to add wherein concentration be 18% tanning solution, addition is 2% of collected trapped fluid volume, mixes, and leaves standstill 5 hours; With 100 object filter-cloth filterings, filter residue discards, and collects filtrate; The hyperfiltration film of selecting molecular weight cut-off 20000, carries out hyperfiltration to the filtrate of collecting, and supplements and add distilled water or pure water wherein; Discard the liquid that sees through in ultra-filtration process, collect trapped fluid, and spray dry with Highspeedcentrifugingandsprayingdrier to it; Spraying is dry, and condition is: 130 DEG C of import hot blast temperatures, export 60 DEG C, and the spray velocity of feed liquid is: 5L/h; Collect the dry gained dry powder of spraying, extract degreasing with supercritical carbon dioxide extraction apparatus; Extraction degreasing, condition is: dry powder loading amount 500g, extraction kettle pressure 15Mp, extraction kettle temperature room temperature to 40 DEG C, separating still pressure 5Mp, separating still temperature room temperature to 40 DEG C, carbon dioxide flow 20L/h, extraction time 0.5h; The component being extracted with carbonic acid gas, for extracting Sea Cucumber Glycosides research; The solid ingredient staying in extraction kettle, with 70% spirituous solution washing, continues to use after the alcohol slops after washing reclaims; Solids component after washing, is placed in vacuum-drying and is dried; Drying conditions is: 30 DEG C of temperature, the absolute pressure 100p in dry epoch, 5 hours time of drying; After dry, gained faint yellow solid is the sea cucumber polysaccharide product of extraction, and wherein sea cucumber polysaccharide content is 80-90%.
Embodiment 3, selects the hyperfiltration film of molecular weight cut-off 80000, and the boiled sea cucumber juice of collecting is carried out to hyperfiltration, and supplements and add distilled water or pure water wherein; Discard the liquid that sees through in ultra-filtration process, collect trapped fluid, and to add wherein concentration be 20% tanning solution, addition is 10% of collected trapped fluid volume, mixes, and leaves standstill 20 hours; With 100 object filter-cloth filterings, filter residue discards, and collects filtrate; The hyperfiltration film of selecting molecular weight cut-off 80000, carries out hyperfiltration to the filtrate of collecting, and supplements and add distilled water or pure water wherein; Discard the liquid that sees through in ultra-filtration process, collect trapped fluid, and spray dry with Highspeedcentrifugingandsprayingdrier to it; Spraying is dry, and condition is: 180 DEG C of import hot blast temperatures, export 80 DEG C, and the spray velocity of feed liquid is: 15L/h; Collect the dry gained dry powder of spraying, extract degreasing with supercritical carbon dioxide extraction apparatus; Extraction degreasing, condition is: dry powder loading amount 1500g, extraction kettle pressure 30Mp, extraction kettle temperature room temperature to 40 DEG C, separating still pressure 20Mp, separating still temperature room temperature to 60 DEG C, carbon dioxide flow 30L/h, extraction time 2h; The component being extracted with carbonic acid gas, for extracting Sea Cucumber Glycosides research; The solid ingredient staying in extraction kettle, with 90% spirituous solution washing, continues to use after the alcohol slops after washing reclaims; Solids component after washing, is placed in vacuum-drying and is dried; Drying conditions is: temperature 50 C, the absolute pressure 5000p in dry epoch, 1 hour time of drying; After dry, gained faint yellow solid is the sea cucumber polysaccharide product of extraction, and wherein sea cucumber polysaccharide content is 80-90%.
Claims (4)
1. boiled sea cucumber juice extracts the method for sea cucumber polysaccharide, it is characterized in that, comprises the steps:
A hyperfiltration, selects the hyperfiltration film of molecular weight cut-off 20000-80000, and the boiled sea cucumber juice of collecting is carried out to hyperfiltration, and supplements and add distilled water or pure water wherein;
B staticly settles, and discards the liquid that sees through in ultra-filtration process, collect trapped fluid, and to add wherein concentration is the tanning solution of 18-20%, and addition is the 2-10% of collected trapped fluid volume, mixes, and leaves standstill 5-20 hour;
C filters, and with 100 object filter-cloth filterings, filter residue discards, and collects filtrate;
D ultra micro membrane sepn, selects the hyperfiltration film of molecular weight cut-off 20000-80000, and the filtrate of collecting is carried out to hyperfiltration, and supplements and add distilled water or pure water wherein;
E spraying is dry, discards the liquid that sees through in ultra-filtration process, collects trapped fluid, and sprays dry with Highspeedcentrifugingandsprayingdrier to it;
F supercritical extraction, collects the dry gained dry powder of spraying, extracts degreasing with supercritical carbon dioxide extraction apparatus; The component being extracted with carbonic acid gas, for extracting Sea Cucumber Glycosides research;
G vacuum-drying, the solid ingredient staying in extraction kettle, with the spirituous solution washing of 70-90%, continues to use after the alcohol slops after washing reclaims; Solids component after washing, is placed in vacuum-drying and is dried;
H sea cucumber polysaccharide product, dry rear gained faint yellow solid is the sea cucumber polysaccharide product of extraction, and wherein sea cucumber polysaccharide content is 80-90%.
2. boiled sea cucumber juice according to claim 1 extracts the method for sea cucumber polysaccharide, it is characterized in that, the spraying described in e step is dry, and condition is: import hot blast temperature 130-180 DEG C, and outlet 60-80 DEG C, the spray velocity of feed liquid is: 5-15L/h.
3. boiled sea cucumber juice according to claim 1 extracts the method for sea cucumber polysaccharide, it is characterized in that, extraction degreasing described in f step, condition is: dry powder loading amount 500-1500g, extraction kettle pressure 15-30Mp, extraction kettle temperature room temperature to 40 DEG C, separating still pressure 5-20Mp, separating still temperature room temperature is to 40-60 DEG C, carbon dioxide flow 20-30L/h, extraction time 0.5-2h.
4. boiled sea cucumber juice according to claim 1 extracts the method for sea cucumber polysaccharide, it is characterized in that, dry described in g step, condition is: temperature 30-50 DEG C, the absolute pressure 100-5000p in dry epoch, time of drying 1-5 hour.
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| CN105884921A (en) * | 2014-11-26 | 2016-08-24 | 卢卫红 | Membrane separation method of sea cucumber polysaccharide fragments acting on simulation space heavy ion radiation oxidation stress |
| CN110590967A (en) * | 2019-08-27 | 2019-12-20 | 中国海洋大学 | Method for recovering organic matters rich in sea cucumber polysaccharide from sea cucumber blanching liquid |
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