CN102048172A - Novel squid ink melanin chelate iron preparation method and application of method - Google Patents
Novel squid ink melanin chelate iron preparation method and application of method Download PDFInfo
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- CN102048172A CN102048172A CN201010516714XA CN201010516714A CN102048172A CN 102048172 A CN102048172 A CN 102048172A CN 201010516714X A CN201010516714X A CN 201010516714XA CN 201010516714 A CN201010516714 A CN 201010516714A CN 102048172 A CN102048172 A CN 102048172A
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- squid ink
- black pigment
- squid
- melanin
- iron
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Abstract
The invention relates to a novel squid ink melanin chelate iron preparation method and the application of the method in preparing anemia and iron deficiency anemia adjuvant therapy health food, functional food or medicines. The method is characterized by the following steps: melanin is separated from the squid ink firstly; the squid ink melanin is added into a buffer solution containing ferrous ions after vacuum freeze drying; the buffer solution is stirred for 8 to 24 hours under the temperature of 4 DEG C to 25 DEG C with the pH value regulated to 5 to 6; 3000-5000*g centrifugal collection for precipitation is carried out under the room temperature; then the precipitate is repeatedly washed by distilled water, and 3000-5000*g centrifugal collection for precipitation and vacuum freeze drying are conducted. The squid ink melanin chelate iron compound prepared through adopting the method utilizes rich and available raw materials and has extremely high melanin content. The method provided by the invention has the advantages of simple procedures, easiness in control, less equipment investment, no environmental pollution, high product yield, etc., and is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method and the application in preparation supplemental treatment anaemia health food, functional food or medicine thereof of novel squid ink black pigment chelated iron.
Background technology
Chinese residents nutrition survey result showed in 2002, China resident anaemia illness rate average out to 15.2%; 2 years old with interior infant, old man, women of child-bearing age's anaemia illness rate are respectively 24.2%, 21.5% and 20.6% more than 60 years old.Pregnant woman's 30% anaemia, pregnant latter stage is higher.Anaemia generally can be divided into and lack the non-nutritive anaemia two big classes that alimentary anemia that iron or cobalamin cause and hemopoietic system dysfunction etc. cause, wherein, in the alimentary anemia mainly based on hypoferric anemia.The chalybeate kind that is used to mend iron is a lot, and commonly used have ferrous sulfate, ferrous fumarate, ferrous gluconate, ferrous succinate, a Nu-Iron etc.It is generally obvious to gastrointestinal tract mucous stimulation that but low molecule is mended chalybeate, so application at present such as Nu-Iron is more.In addition, have not yet to see all effective single component products of auxiliary improvement anaemia of non-nutritive anaemia that alimentary anemia and hemopoietic system dysfunction etc. is caused.
Squid is Mollusca, Cephalopoda, squid section aquatic/marine animals.It is reported that the year amount of fishing of whole world squid reaches 4,000,000 tons, China is one of the highest country of whole world amount of fishing.In the process of squid, most of processing factories are discarded with the squid ink sac, caused environmental pollution, and squid ink sac abundant raw material is easy to get, and are badly in need of seeking for it the effectively outlet of utilization.Squid ink sac main component is melanin and proteoglycan complex, and melanic content is about 20% in the bright prepared Chinese ink, is the eumelanin of the condensate formation of a class istain.Squid ink black pigment under certain condition can with the iron ion chela and, chela and ability increase with pH and rise, optimal pH is 5-6, the pH value is 4 when following, the iron ion chelation percent is lower than 50%.But, at present because the defective on the method, pH forms the ferric hydroxide precipitate of slightly solubility easily greater than 4 o'clock iron ions, be difficult to control in the production process, therefore can not realize suitability for industrialized production, demand urgently developing and a kind ofly can realize preparation method suitability for industrialized production, high Fe contained squid ink black pigment chelated iron compound.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and the application in health food, functional food or the medicine of preparation supplemental treatment anaemia and hypoferric anemia thereof of novel squid ink black pigment chelated iron, to remedy the above-mentioned deficiency of prior art.
A kind of preparation method of novel squid ink black pigment chelated iron, it is characterized in that from squid prepared Chinese ink, isolating melanin earlier, after the vacuum freeze drying, again squid ink black pigment is added and contain in the cushioning liquid of iron ion, regulate pH to 5-6,4 ℃-25 ℃ were stirred 8-24 hour down, afterwards 3000-5000 * g centrifugal collecting precipitation at room temperature, at last with 3000-5000 * g centrifugal collecting precipitation under gained sediment distilled water cyclic washing, the room temperature, vacuum freeze drying.
The application of above-mentioned novel squid ink black pigment chelated iron in health food, functional food or the medicine of preparation supplemental treatment hypoferric anemia and functional anaemia.
The squid ink black pigment chelated iron compound of the present invention preparation, the abundant raw material of employing is easy to get, melanin content is high, and have step simple, be easy to control, equipment investment is few, non-environmental-pollution, product yield advantages of higher, is suitable for suitability for industrialized production.
The specific embodiment
During preparation squid ink black pigment chelated iron, earlier from squid prepared Chinese ink, isolate melanin, after the vacuum freeze drying, again squid ink black pigment is added and contain in the cushioning liquid of iron ion, regulate pH to 5-6,4 ℃-25 ℃ were stirred 8-24 hour down, afterwards 3000-5000 * g centrifugal collecting precipitation at room temperature, at last with 3000-5000 * g centrifugal collecting precipitation under gained sediment distilled water cyclic washing, the room temperature, vacuum freeze drying.
Embodiment: take by weighing 1Kg North Pacific squid prepared Chinese ink and isolate the about 200g of squid ink black pigment, take by weighing 20g, after the vacuum freeze drying, add 5L and contain 10mM FeCl
350mM sodium acetate buffer solution in, regulate pH to 6.0,4 ℃ are stirred down, and squid ink black pigment is evenly disperseed, and stir 12h; Collect gained solution, 4000 * g centrifugal collecting precipitation under the room temperature; At last with the gained sediment through distilled water cyclic washing and centrifugal collecting precipitation 3 times, remove not in conjunction with iron ion, with gained sediment vacuum freeze drying, obtain the squid ink black pigment chelated iron.By analysis, this product is the heteropolymer chelated iron based on indole structure, and purity is 89.2%, and iron-holder is 75mg/g.
In the present embodiment, described North Pacific squid can change Peru squid, red squid, Argentinian squid or New Zealand squid into, all can obtain similar effects.The purity of the squid ink black pigment chelated iron of the present invention's preparation is 70%-99%, and iron-holder is 40mg-90mg/g.Described buffer solution can be used Tri(Hydroxymethyl) Amino Methane Hydrochloride, carbonate or phosphate solution instead; Described FeCl
3Can use Fe instead
2(S0
4)
3, FeCl
2Or FeS0
4Deng the salt that can form the soluble iron ion, concentration is 0.5-10mM.
The novel squid ink black pigment chelated iron of the present invention preparation can be used as the health food for the treatment of hypoferric anemia and functional anaemia simultaneously and the active ingredient of related drugs, according to health care and treatment needs, can make several formulations with edible and pharmaceutic adjuvant.
Below novel squid ink black pigment chelated iron supplemental treatment and the effect that improves anaemia are further described:
One. the pharmacodynamic study of novel squid ink black pigment chelated iron
1. prove by zoopery that the squid ink black pigment chelated iron that makes has the significant hypoferric anemia activity of improving.The hypoferric anemia rat model is adopted in experiment in the body.The Wistar rat is divided into 6 groups at random, and the 1-2 group is respectively normal and model control group; The 3rd group of positive control group (FeCl
2), irritate stomach Fe
2+2mg/kg BW; The 4-6 group is irritated stomach respectively and is equivalent to Fe for squid ink black pigment chelated iron group
2+0.5,1,2mg/kg BW, 1 time/d, continuous 21d; The tail vein was got blood after last was irritated stomach, measured quantity of leucocyte (WBC), erythrocyte number (RBC), serum levels of iron (SI), free protoporphyrin (FEP), hemoglobin (HGB), packed cell volume (HCT), mean corpuscular volume (MCV) (MCV), mean corpuscular hemoglobin (MCH).The results are shown in Table 1, novel squid ink black pigment chelated iron can significantly improve hypoferric anemia rat S worker, FEP, HGB, HCT, MCV, MCH level, show that the squid ink black pigment chelated iron has the effect of the hypoferric anemia of improvement, when 0.5mg/kg dosage, can reach FeCl with 2mg/kg
2The effect that is equal to; Squid ink black pigment chelated iron treated animal serum levels of iron content is with amount FeCl
2Group improves 1.5 times, shows the FeCl of the absorptivity of novel squid ink black pigment chelated iron apparently higher than inorganic iron
2In addition, novel squid ink black pigment chelated iron can significantly improve the reduction of body weight that the rat hypoferric anemia caused, liver weight and increase haemocyte quantity, and the alimentary canal of animal is stimulated than FeCl
2Little, the results are shown in Table 2.Above result proves that novel squid ink black pigment chelated iron significantly is better than conventional benefit chalybeate FeCl to the result of treatment of hypoferric anemia
2
The novel squid ink black pigment chelated iron of table 1 to the influence of the every index of hypoferric anemia rat (n=10,
)
Annotate:
△Compare with the normal control group P＜0.01;
*Compare with model control group P＜0.01
The novel squid ink black pigment chelated iron of table 2 to the influence of hypoferric anemia rat serum cell quantity, body weight and liver weight (n=10,
)
Annotate:
△Compare with the normal control group P＜0.05;
*Compare with model control group P＜0.05
2. adopt marrow hemopoiesis damage model mouse to prove, the effect that the novel squid ink black pigment chelated iron of the present invention's preparation has the functional anaemia of significant improvement.With 100,300 and 900mg/kg BW squid ink black pigment chelated iron irritate stomach caused by cyclophosphamide marrow hemopoiesis damage model mouse respectively, the results are shown in Table 3.The result shows; novel squid ink black pigment chelated iron has significant antagonism and promotes restitution the minimizing of bone marrow nucleated cell (BMNC), candidate stem cell (CFU-S), grain monosystem CFU-GM (CFU-GM) and the peripheral red blood cells quantity of bone marrow injury model mice, illustrates that the prepared novel squid ink black pigment chelated iron of the present invention has good preventing, protection and therapeutic action to functional anaemia.
The novel squid ink black pigment chelated iron of table 3 to the exercising result of caused by cyclophosphamide marrow hemopoiesis damage model mouse (n=10,
)
Annotate:
△Compare with the normal control group P＜0.01;
*P＜0.05,
*Compare with model control group P＜0.01
Two. the safety experiment of novel squid ink black pigment chelated iron
To the disposable squid ink black pigment chelated iron that gavages various dose of ICR mouse (0.464,1.00,2.15,4.64g/kg), behind the 14d, each dosage treated animal does not all have death, and there is not any abnormal behavior, body weight does not have and rises appreciably routine blood test, liver, the every inspection of kidney merit, no significant difference, the histopathologic examination of animal viscera is no abnormal, shows that novel squid ink black pigment chelated iron has no side effect and do not have cumulative toxicity.
Three. the stability of novel squid ink black pigment chelated iron
The novel squid ink black pigment chelated iron of the present invention preparation was preserved 12-18 month at normal temperatures, the experiment proved that its biologically active do not have obvious reduction.
Claims (3)
1. the preparation method of a novel squid ink black pigment chelated iron, it is characterized in that from squid prepared Chinese ink, isolating melanin earlier, after the vacuum freeze drying, again squid ink black pigment is added and contain in the cushioning liquid of iron ion, regulate pH to 5-6,4 ℃-25 ℃ were stirred 8-24 hour down, afterwards 3000-5000 * g centrifugal collecting precipitation at room temperature, at last with 3000-5000 * g centrifugal collecting precipitation under gained sediment distilled water cyclic washing, the room temperature, vacuum freeze drying.
2. the preparation method of novel according to claim 1 squid ink black pigment chelated iron is characterized in that described iron ion buffer solution is for containing FeCl
3, Fe
2(SO
4)
3, FeCl
2Or FeSO
4Acetate, Tri(Hydroxymethyl) Amino Methane Hydrochloride, carbonate or phosphatic cushioning liquid.
3. the application of the described novel squid ink black pigment chelated iron of claim 1 in preparation supplemental treatment hypoferric anemia and functional anaemia health food, functional food or medicine.
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|---|---|---|---|
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| CN102048172B CN102048172B (en) | 2013-05-22 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108014136A (en) * | 2017-09-21 | 2018-05-11 | 浙江海洋大学 | A kind of preparation and application of squid ink black pigment chelating calcium tablet |
| CN109481470A (en) * | 2019-01-08 | 2019-03-19 | 广东海洋大学 | A kind of preparation method of fish blood source iron supplementary |
| CN111990650A (en) * | 2020-08-13 | 2020-11-27 | 自然资源部第三海洋研究所 | Preparation method and application of squid natural melanin chelated chromium (III) salt |
| CN113875990A (en) * | 2021-10-11 | 2022-01-04 | 中北大学 | Ferrous iron with antioxidant activity and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015355A (en) * | 2007-02-13 | 2007-08-15 | 中国海洋大学 | Preparing method of squid melanin iron and application thereof |
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2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015355A (en) * | 2007-02-13 | 2007-08-15 | 中国海洋大学 | Preparing method of squid melanin iron and application thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108014136A (en) * | 2017-09-21 | 2018-05-11 | 浙江海洋大学 | A kind of preparation and application of squid ink black pigment chelating calcium tablet |
| CN108014136B (en) * | 2017-09-21 | 2020-07-24 | 浙江海洋大学 | Preparation and application of squid ink melanin-chelated calcium tablets |
| CN109481470A (en) * | 2019-01-08 | 2019-03-19 | 广东海洋大学 | A kind of preparation method of fish blood source iron supplementary |
| CN111990650A (en) * | 2020-08-13 | 2020-11-27 | 自然资源部第三海洋研究所 | Preparation method and application of squid natural melanin chelated chromium (III) salt |
| CN111990650B (en) * | 2020-08-13 | 2023-03-10 | 自然资源部第三海洋研究所 | Preparation method and application of squid natural melanin chelated chromium (III) salt |
| CN113875990A (en) * | 2021-10-11 | 2022-01-04 | 中北大学 | Ferrous iron with antioxidant activity and preparation method thereof |
| CN113875990B (en) * | 2021-10-11 | 2024-06-11 | 中北大学 | Ferrous melanin with antioxidant activity and preparation method thereof |
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|---|---|
| CN102048172B (en) | 2013-05-22 |
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