CN101643430A - Method for extracting seaweed organic iodine from seaweed or seaweed root - Google Patents
Method for extracting seaweed organic iodine from seaweed or seaweed root Download PDFInfo
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- CN101643430A CN101643430A CN200910017649A CN200910017649A CN101643430A CN 101643430 A CN101643430 A CN 101643430A CN 200910017649 A CN200910017649 A CN 200910017649A CN 200910017649 A CN200910017649 A CN 200910017649A CN 101643430 A CN101643430 A CN 101643430A
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 44
- 239000011630 iodine Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 21
- 241001474374 Blennius Species 0.000 title abstract 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000007710 freezing Methods 0.000 claims abstract description 6
- 230000008014 freezing Effects 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims description 25
- 238000001556 precipitation Methods 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 13
- 238000004108 freeze drying Methods 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 241000512259 Ascophyllum nodosum Species 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- NYPYHUZRZVSYKL-ZETCQYMHSA-N 3,5-diiodo-L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC(I)=C(O)C(I)=C1 NYPYHUZRZVSYKL-ZETCQYMHSA-N 0.000 claims description 6
- 235000010443 alginic acid Nutrition 0.000 claims description 6
- 229920000615 alginic acid Polymers 0.000 claims description 6
- 229960000415 diiodotyrosine Drugs 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 5
- 239000004278 EU approved seasoning Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 206010020772 Hypertension Diseases 0.000 claims description 5
- 229930195725 Mannitol Natural products 0.000 claims description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 5
- 230000002411 adverse Effects 0.000 claims description 5
- 238000005352 clarification Methods 0.000 claims description 5
- PXEDJBXQKAGXNJ-QTNFYWBSSA-L disodium L-glutamate Chemical class [Na+].[Na+].[O-]C(=O)[C@@H](N)CCC([O-])=O PXEDJBXQKAGXNJ-QTNFYWBSSA-L 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 235000013305 food Nutrition 0.000 claims description 5
- 235000011194 food seasoning agent Nutrition 0.000 claims description 5
- 230000001631 hypertensive effect Effects 0.000 claims description 5
- 208000017169 kidney disease Diseases 0.000 claims description 5
- 235000010355 mannitol Nutrition 0.000 claims description 5
- 239000000594 mannitol Substances 0.000 claims description 5
- 238000001471 micro-filtration Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 235000013923 monosodium glutamate Nutrition 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 230000033764 rhythmic process Effects 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910001415 sodium ion Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 238000003672 processing method Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 13
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 6
- 231100000331 toxic Toxicity 0.000 description 5
- 230000002588 toxic effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 102000011759 adducin Human genes 0.000 description 3
- 108010076723 adducin Proteins 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229910001410 inorganic ion Inorganic materials 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 101000800133 Homo sapiens Thyroglobulin Proteins 0.000 description 1
- 206010020850 Hyperthyroidism Diseases 0.000 description 1
- 206010067997 Iodine deficiency Diseases 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 241000607768 Shigella Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 241000193996 Streptococcus pyogenes Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 102000047688 human TG Human genes 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 235000006479 iodine deficiency Nutrition 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Edible Seaweed (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for extracting seaweed organic iodine from seaweed or a seaweed root, which is characterized by comprising the following technical steps: washing and soaking raw materials, extracting leaching liquor and adding alcohol to extract supernate; recovering the alcohol, adjusting the pH value and separating the supernate; and freezing and drying muddy liquid at the bottom in vacuum to obtain the product. The product has high purity and favorable water-based rehabilitation and is quite convenient to apply; and the processing method is simple, convenient and easy.
Description
Technical field:
The present invention relates to the sea-tangle processing technique field, is a kind of method of extracting the sea-tangle organic iodine from sea-tangle or Radix Laminariae specifically, adopts technology such as isoelectric precipitation, vacuum lyophilization.
Background technology:
It is micro-that iodine is that a kind of human body must get, and iodine deficiency will cause a series of serious diseases.The methods to supply iodine that generally adopts both at home and abroad mainly is the supply iodized salt at present.Used idodine mainly is KIO in the salt compounded of iodine production
3And KI, that China adopts at present mainly is KIO
3Though these two kinds of idodine have played certain effect of enriching the iodine, and all have certain defective.The human absorptivity of KI compares KIO
3Good, but the character instability in processing, transportation storage, is seen the volatile loss of light chance thermal capacitance, especially in the cooking process, loses even more serious.To the human consumer when edible, human body has only absorbed and has been consolidated in the salt iodometricly about 10%, and the iodine that really absorbs human body has only about 3% of amount of reinforcement; KIO
3Character is more stable than KI, sees to be heated light be not easy can lose.But it is low in the intravital absorption trans-utilization of people rate, and toxic side effect is apparent in view.In the last few years, the clinical medicine worker and the endemy worker of internal secretion aspect investigated discovery, used KIO
3After replacing KI to produce salt compounded of iodine, though iodine deficient area crowd Medianofurinaryiodine compliance rate has improved, crowd's goitrerate does not have corresponding reduction, and that iodine causes disease such as hyperthyroidism is in rising trend.Show KIO
3Salt compounded of iodine enriches the iodine, and is unsatisfactory to the swollen elimination of first effect, and its toxic side effect is apparent in view.
Well-known sea-tangle is to contain the abundantest biology of iodine on the earth, and amount of iodine is the high quality raw material that extract iodine up to 5000-7000mg/kg.Iodine in the sea-tangle is divided into two kinds, and a kind of is inorganic iodine, and another kind is an organic iodine.Organic iodine in the sea-tangle mainly is an iodogorgoic acid, and it is the plain synthetic precursor of human thyroglobulin.Has inorganic iodine-replenishing agent KIO
3With the unrivaled advantage of KI, character is highly stable, even under 270 ℃, and still non-volatile loss; Safe, there is not toxic side effect, even exceed 100 times of convention amounts, there is not toxic side effect yet; The absorption of human body utilization ratio is up to 80%.People continually develop the method for extracting organic iodine from sea-tangle, but the organic iodine poor practicability of extracting, as Chinese patent zL00111384.4, denomination of invention: a kind of method of from sea-tangle, extracting active iodine, there is following drawback in this method: 1) employing zwitterion exchange absorption method removes the inorganic salts in the extracting solution, because inorganic ion content height in the kelp extract, active iodine content is low, thereby ion exchange resin is very easily saturated, removal efficiency is low, the active iodine purity that makes is low, and content has only about 15%, when being used for salt compounded of iodine production, bring a certain amount of impurity into, influence the quality of salt compounded of iodine; 2) since in the kelp extract inorganic ion content height, ion exchange resin very easily saturated, keep certain production efficiency, need be through a large amount of acid-base solution commonly used, the resin that repetitive scrubbing regeneration is saturated, thereby produce a large amount of acid-base waste fluids, as not treated discharging, with serious environment pollution; If handle back up to standard discharging, then the production cost increase is very big, and benefit is lower; 3) in order to remove the algin in the extracting solution, macromolecular substance such as protein, with the inorganic salt small molecules, adopt the multistage gradient ultra micro membrane filter plant of molecular weight cut-off 80,000-400, when especially using molecular weight cut-off and be the membrane module of committed step of 400-1000, because the aperture of film is very little, need filter pressure very big, up to 20-30atm, device fabrication requires very high, and the little molecular weight cut-off that arrives of pore size filter is below 1000, no longer be the ultrafiltration scope, and reached the nanofiltration scope, efficient is very low, in order to reach certain production efficiency, need to increase the filtration area of microfilter, facility investment is very big, is not easy to the enforcement of suitability for industrialized production; 4) adopt spraying drying at last, not only energy consumption height, and the product that obtains is influenced by pyritous, and color is dark, the whiteness of the salt that influence is produced in the future; Rehydration is poor, and solubleness is low, needs the water dissolution of volume, remove this part redundant moisture, and salt industry production department need adjust original production line, increases drying process.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of method of utilizing technology such as isoelectric precipitation, vacuum lyophilization to extract the sea-tangle organic iodine from sea-tangle or Radix Laminariae is provided, mainly solve inorganic idodine KI unstable and absorbance difference and idodine KIO in the existing salt compounded of iodine
3Undesirable and its toxic side effect is apparent in view to the swollen effect of eliminating of first, and the dna purity of active iodine is low among the Chinese patent zL00111384.4, wastewater flow rate big, the technology very complicated, production efficiency is low, facility investment is big, be difficult for industrializing implementation and product color deeply, problems such as rehydration difference.
In order to achieve the above object, the present invention is achieved in that a kind of method of extracting the sea-tangle organic iodine from sea-tangle or Radix Laminariae, and its special character is that it comprises following processing step:
The a cleaning and dipping: choose drying sea-tangle or Radix Laminariae, clean, remove impurity such as silt, dry, sea-tangle adds sea-tangle weight 10-25 pure water doubly, and Radix Laminariae adds Radix Laminariae weight 5-8 pure water doubly, soaks 5-20h under the room temperature;
B extracts vat liquor: after vat liquor filters through plate-and-frame filter press, and gained solution clear, color is pale brown; Pass through again after the tubular fibre membrane microfiltration of molecular weight cut-off 20000-50000, become light yellow transparent solution; With the high pressure steam of this liquid with 4-5kg/cm2, rapid heating is boiled 2-3h, adopts the adverse current refrigerating unit, is chilled to room temperature fast; After leaving standstill 4-5h, siphon goes out supernatant liquor, and the turbid solution of bottom adopts plate-and-frame filter press to filter, and removes precipitation; The clear liquid that gained filtrate and siphon go out merges;
Sea-tangle behind the extraction organic iodine can perhaps be used to produce kelp food as the raw material that extracts algin;
C adds ethanol and puts on clear liquid: in this liquid, add liquid volume 3-5 95% edible ethanol doubly slowly, stir while adding, leave standstill clarification 4-5h; Supernatant liquor is collected in siphon, and the turbid solution of bottom filters with plate-and-frame filter press, removes precipitation; The clear liquid that gained filtrate and siphon go out merges standby;
D recovered alcohol adjust pH: with this clear liquid recovery of alcohol distillation, alcohol recycle; Liquid in the still kettle, be cooled to room temperature after, transfer pH to 5.0-5.3 with dilute hydrochloric acid, promptly near the iso-electric point of sea-tangle organic iodine iodogorgoic acid, staticly settle 4-5h;
E isolates supernatant liquor: supernatant liquor is isolated in siphon, heating is concentrated into dried, 95% edible ethanol dissolving with 60 ℃, supernatant liquor is collected in siphon, cools off below this clear liquid to 10 ℃, has alabastrine crystallization to separate out, collect this crystallization, after the drying, be medical N.F,USP MANNITOL raw material, purity can reach more than 95%; Ethanol in this step, distillation is recycled; Not by 60 ℃ 95% edible ethanol dissolved solid substance, contain compositions such as a large amount of Sodium Glutamates, KCl, especially wherein KCl has the effect that reduces the rhythm of the heart, offsets sodium ion in the salt, can be used as hypertensive patient, nephropathy patient's low-sodium healthcare seasonings;
The f product: the turbid solution of bottom, use link-suspended basket centrifuge, centrifugal treating is separated 30min, collecting precipitation under 2000rpm; Precipitation is put in freezing 20-40min in-30 ℃ of low temperature refrigerators, moves in vacuum freeze drier (FD), under 15-25 ℃, absolute pressure 5-10Pa condition, freeze-drying 20-30h, water content≤5-8% in product after the freeze-drying promptly gets product.
A kind of method of extracting the sea-tangle organic iodine from sea-tangle or Radix Laminariae of the present invention, its described plate-and-frame filter press is with 100 purpose filter clothes.
Compared with the prior art a kind of method of extracting the sea-tangle organic iodine from sea-tangle or Radix Laminariae of the present invention has outstanding substantive distinguishing features and marked improvement, and 1, this method product purity height of utilizing isoelectric precipitation to make, the production efficiency height, simple to operate; 2, adopt the product rehydration of vacuum lyophilization good, use very convenient; 3, this method has not only been extracted the sea-tangle organic iodine, and has avoided the generation of the three-waste pollution in the processing; 4, facility investment is few, and production cost is low, high efficiency, and help realizing suitability for industrialized production.
Embodiment:
In order to understand better and to implement, describe a kind of method of from sea-tangle or Radix Laminariae, extracting the sea-tangle organic iodine of the present invention in detail below in conjunction with embodiment.
Embodiment 1, choose drying sea-tangle as required, clean, remove impurity such as silt, after drying, add the pure water of 17.5 times of sea-tangle weight, soak 12.5h under the room temperature, after vat liquor filtered through 100 purpose plate-and-frame filter press, gained solution clear, color is pale brown, passes through after the tubular fibre membrane microfiltration of molecular weight cut-off 20000-50000 again, become light yellow transparent solution, with the high pressure steam of this liquid with 4.5kg/cm2, rapid heating is boiled 2.5h, adopts the adverse current refrigerating unit, be chilled to room temperature fast, after leaving standstill 4.5h, siphon goes out supernatant liquor, and the turbid solution of bottom adopts 100 purpose plate-and-frame filter press to filter, remove precipitation, the clear liquid that gained filtrate and siphon go out merges; Sea-tangle behind the extraction organic iodine can perhaps be used to produce kelp food as the raw material that extracts algin; In aforesaid liquid, add 95% edible ethanol of 3.5 times of liquid volumes slowly, stir while adding, leave standstill clarification 4.5h; Supernatant liquor is collected in siphon, and the turbid solution of bottom filters with 100 purpose plate-and-frame filter press, removes precipitation, and the clear liquid that supernatant liquor and siphon go out merges, with this clear liquid recovery of alcohol distillation, alcohol recycle; Liquid in the still kettle, be cooled to room temperature after, transfer pH to 5.2 with dilute hydrochloric acid, promptly near the iso-electric point of sea-tangle organic iodine iodogorgoic acid, staticly settle 4.5h;
Supernatant liquor is isolated in siphon, and heating is concentrated into dried, and with 60 ℃ 95% edible ethanol dissolving, siphon goes out supernatant liquor, cool off below this clear liquid to 10 ℃, have alabastrine crystallization to separate out, collect this crystallization, after the drying, be medical N.F,USP MANNITOL raw material, purity can reach more than 95%; Ethanol in this step, distillation is recycled; Not by 60 ℃ 95% edible ethanol dissolved solid substance, contain compositions such as a large amount of Sodium Glutamates, KCl, especially wherein KCl has the effect that reduces the rhythm of the heart, offsets sodium ion in the salt, can be used as hypertensive patient, nephropathy patient's low-sodium healthcare seasonings;
The turbid solution of bottom is used link-suspended basket centrifuge, and centrifugal treating is separated 30min, collecting precipitation under 2000rpm; Precipitation is put in freezing 30min in-30 ℃ of low temperature refrigerators, moves in vacuum freeze drier (FD), under 20 ℃, absolute pressure 7.5Pa condition, freeze-drying 25h, water content≤5-8% in product after the freeze-drying promptly gets product.
The proterties and the performance testing index of the product that aforesaid method makes are as follows:
1, product proterties:
Table 1:
| Project | Proterties and index |
| Sensory properties | White has the peculiar delicate fragrance of light sea-tangle, free from extraneous odour to pale yellow powder; |
| Solvability | Soluble in water and spirituous solution is colourless transparent solution; Solubleness 〉=10g/100ml in the water; Be insoluble in organic solvents such as ether |
2, product physical and chemical index:
| Project | Unit | Index | Remarks |
| Total iodine | ??mg/kg | ??≥3×10 5 | |
| Inorganic iodine | ??mg/kg | ??≤80 | |
| Arsenic | ??mg/kg | ??≤2.0 | |
| Plumbous | ??mg/kg | ??≤2.0 | |
| Heavy metal | ??mg/kg | ??≤10 | In lead |
3, product Biological indicators:
| Project | Unit | Index |
| Total number of bacterial colony | ??cfu/g | ??＜10 |
| Coliform | ??MPN/100g | ??＜30 |
| Salmonella | Must not detect | |
| Shigella | Must not detect | |
| Streptococcus hemolyticus | Must not detect | |
| Streptococcus aureus | Must not detect | |
| Mould | ??cfu/g | ??＜10 |
| Yeast | ??cfu/g | ??＜10 |
Embodiment 2, choose drying sea-tangle as required, impurity such as silt are removed in cleaning, after drying, add the pure water of 10 times of sea-tangle weight, soak 20h under the room temperature, after vat liquor filters through 100 purpose plate-and-frame filter press, gained solution clear, color is pale brown, pass through again after the tubular fibre membrane microfiltration of molecular weight cut-off 20000-50000, become light yellow transparent solution; With the high pressure steam of this liquid with 4kg/cm2, rapid heating is boiled 3h, adopts the adverse current refrigerating unit, be chilled to room temperature fast, leave standstill 4h after, siphon goes out supernatant liquor, the turbid solution of bottom adopts 100 purpose plate-and-frame filter press to filter, and removes precipitation, and the clear liquid that gained filtrate and siphon go out merges; Sea-tangle behind the extraction organic iodine can perhaps be used to produce kelp food as the raw material that extracts algin; In aforesaid liquid, add 95% edible ethanol of 3 times of liquid volumes slowly, stir while adding, leave standstill clarification 5h; Supernatant liquor is collected in siphon, and the turbid solution of bottom filters with 100 purpose plate-and-frame filter press, removes precipitation, and the clear liquid that supernatant liquor and siphon go out merges, with this clear liquid recovery of alcohol distillation, alcohol recycle; With the liquid in the still kettle, be cooled to room temperature after, transfer pH to 5.0 with dilute hydrochloric acid, promptly near the iso-electric point of sea-tangle organic iodine iodogorgoic acid, staticly settle 4h;
Supernatant liquor is isolated in siphon, and heating is concentrated into dried, and with 60 ℃ 95% edible ethanol dissolving, siphon goes out supernatant liquor, cool off below this clear liquid to 10 ℃, have alabastrine crystallization to separate out, collect this crystallization, after the drying, be medical N.F,USP MANNITOL raw material, purity can reach more than 95%; Ethanol in this step, distillation is recycled; Not by 60 ℃ 95% edible ethanol dissolved solid substance, contain compositions such as a large amount of Sodium Glutamates, KCl, especially wherein KCl has the effect that reduces the rhythm of the heart, offsets sodium ion in the salt, can be used as hypertensive patient, nephropathy patient's low-sodium healthcare seasonings;
The turbid solution of bottom is used link-suspended basket centrifuge, and centrifugal treating is separated 30min, collecting precipitation under 2000rpm; Precipitation is put in freezing 20min in-30 ℃ of low temperature refrigerators, moves in vacuum freeze drier (FD), under 15 ℃, absolute pressure 10Pa condition, freeze-drying 30h, water content≤5-8% in product after the freeze-drying promptly gets product of the present invention.
Embodiment 3, choose drying sea-tangle as required, clean, and remove impurity such as silt, after drying, add the pure water of 25 times of sea-tangle weight, soak 5h under the room temperature, after vat liquor filters through 100 purpose plate-and-frame filter press, and gained solution clear, color is pale brown; Pass through again after the tubular fibre membrane microfiltration of molecular weight cut-off 20000-50000, become light yellow transparent solution; With the high pressure steam of this liquid with 5kg/cm2, rapid heating is boiled 2h, adopts the adverse current refrigerating unit, is chilled to room temperature fast; After leaving standstill 5h, siphon goes out supernatant liquor, and the turbid solution of bottom adopts 100 purpose plate-and-frame filter press to filter, and removes precipitation, and the clear liquid that gained filtrate and siphon go out merges; Sea-tangle behind the extraction organic iodine can perhaps be used to produce kelp food as the raw material that extracts algin; In aforesaid liquid, add 95% edible ethanol of 5 times of liquid volumes slowly, stir while adding, leave standstill clarification 4h, siphon goes out supernatant liquor, and the turbid solution of bottom filters with 100 purpose plate-and-frame filter press, remove precipitation, the clear liquid that supernatant liquor and siphon go out merges, with this clear liquid recovery of alcohol distillation, the alcohol recycle, with the liquid in the still kettle, be cooled to room temperature after, transfer pH to 5.3 with dilute hydrochloric acid, be near the iso-electric point of sea-tangle organic iodine iodogorgoic acid, staticly settle 5h;
Supernatant liquor is isolated in siphon, and heating is concentrated into dried, and with 60 ℃ 95% edible ethanol dissolving, siphon goes out supernatant liquor, cool off below this clear liquid to 10 ℃, have alabastrine crystallization to separate out, collect this crystallization, after the drying, be medical N.F,USP MANNITOL raw material, purity can reach more than 95%; Ethanol in this step, distillation is recycled; Not by 60 ℃ 95% edible ethanol dissolved solid substance, contain compositions such as a large amount of Sodium Glutamates, KCl, especially wherein KCl has the effect that reduces the rhythm of the heart, offsets sodium ion in the salt, can be used as hypertensive patient, nephropathy patient's low-sodium healthcare seasonings;
The turbid solution of bottom is used link-suspended basket centrifuge, and centrifugal treating is separated 30min, collecting precipitation under 2000rpm; Precipitation is put in freezing 30min in-30 ℃ of low temperature refrigerators, moves in vacuum freeze drier (FD), under 20 ℃, absolute pressure 7.5Pa condition, freeze-drying 25h, water content≤5-8% in product after the freeze-drying promptly gets product of the present invention.
Embodiment 4, and with embodiment 1,2 or 3, difference is to choose drying Radix Laminariae, clean, and remove impurity such as silt, after drying, add Radix Laminariae weight 5-8 pure water doubly, soak 5-20h under the room temperature.
Claims (2)
1, a kind of method of extracting the sea-tangle organic iodine from sea-tangle or Radix Laminariae is characterized in that it comprises following processing step:
The a cleaning and dipping: choose drying sea-tangle or Radix Laminariae, clean, remove impurity such as silt, dry, sea-tangle adds sea-tangle weight 10-25 pure water doubly, and Radix Laminariae adds Radix Laminariae weight 5-8 pure water doubly, soaks 5-20h under the room temperature;
B extracts vat liquor: after vat liquor filters through plate-and-frame filter press, and gained solution clear, color is pale brown; Pass through again after the tubular fibre membrane microfiltration of molecular weight cut-off 20000-50000, become light yellow transparent solution; With the high pressure steam of this liquid with 4-5kg/cm2, rapid heating is boiled 2-3h, adopts the adverse current refrigerating unit, is chilled to room temperature fast; After leaving standstill 4-5h, siphon goes out supernatant liquor, and the turbid solution of bottom adopts plate-and-frame filter press to filter, and removes precipitation; The clear liquid that gained filtrate and siphon go out merges;
Sea-tangle behind the extraction organic iodine can perhaps be used to produce kelp food as the raw material that extracts algin;
C adds ethanol and puts on clear liquid: in this liquid, add liquid volume 3-5 95% edible ethanol doubly slowly, stir while adding, leave standstill clarification 4-5h; Supernatant liquor is collected in siphon, and the turbid solution of bottom filters with plate-and-frame filter press, removes precipitation; The clear liquid that gained filtrate and siphon go out merges standby;
D recovered alcohol adjust pH: with this clear liquid recovery of alcohol distillation, alcohol recycle; Liquid in the still kettle, be cooled to room temperature after, transfer pH to 5.0-5.3 with dilute hydrochloric acid, promptly near the iso-electric point of sea-tangle organic iodine iodogorgoic acid, staticly settle 4-5h;
E isolates supernatant liquor: supernatant liquor is isolated in siphon, heating is concentrated into dried, 95% edible ethanol dissolving with 60 ℃, supernatant liquor is collected in siphon, cools off below this clear liquid to 10 ℃, has alabastrine crystallization to separate out, collect this crystallization, after the drying, be medical N.F,USP MANNITOL raw material, purity can reach more than 95%; Ethanol in this step, distillation is recycled; Not by 60 ℃ 95% edible ethanol dissolved solid substance, contain compositions such as a large amount of Sodium Glutamates, KCl, especially wherein KCl has the effect that reduces the rhythm of the heart, offsets sodium ion in the salt, can be used as hypertensive patient, nephropathy patient's low-sodium healthcare seasonings;
The f product: the turbid solution of bottom, use link-suspended basket centrifuge, centrifugal treating is separated 30min, collecting precipitation under 2000rpm; Precipitation is put in freezing 20-40min in-30 ℃ of low temperature refrigerators, moves in vacuum freeze drier (FD), under 15-25 ℃, absolute pressure 5-10Pa condition, freeze-drying 20-30h, water content≤5-8% in product after the freeze-drying promptly gets product.
2, a kind of method of extracting the sea-tangle organic iodine from sea-tangle or Radix Laminariae according to claim 1 is characterized in that described plate-and-frame filter press is with 100 purpose filter clothes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103070431A (en) * | 2012-08-22 | 2013-05-01 | 浙江省海洋开发研究院 | Kelp extract iodine tablet and preparation method thereof |
| CN103704721A (en) * | 2013-12-27 | 2014-04-09 | 王庆忠 | Method for extracting organic iodine from seaweeds and producing organic iodine tablets |
| CN104256252A (en) * | 2014-09-15 | 2015-01-07 | 福建农林大学 | Method for preparing seaweed product for reducing blood pressure via step-by-step extraction and bioconversion coupling |
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| CN1102067C (en) * | 2000-09-26 | 2003-02-26 | 烟台长岛经济开发有限公司 | Process for extracting active iodine from kelp |
| CN100425526C (en) * | 2005-08-18 | 2008-10-15 | 山东寻山水产集团有限公司 | Process for extracting iodine from kelp |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103070431A (en) * | 2012-08-22 | 2013-05-01 | 浙江省海洋开发研究院 | Kelp extract iodine tablet and preparation method thereof |
| CN103070431B (en) * | 2012-08-22 | 2013-11-27 | 浙江省海洋开发研究院 | Kelp extract iodine tablet and preparation method thereof |
| CN103704721A (en) * | 2013-12-27 | 2014-04-09 | 王庆忠 | Method for extracting organic iodine from seaweeds and producing organic iodine tablets |
| CN104256252A (en) * | 2014-09-15 | 2015-01-07 | 福建农林大学 | Method for preparing seaweed product for reducing blood pressure via step-by-step extraction and bioconversion coupling |
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