CN106806383A - A kind of preparation method of pachymaran iron complexes - Google Patents

A kind of preparation method of pachymaran iron complexes Download PDF

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CN106806383A
CN106806383A CN201510838955.9A CN201510838955A CN106806383A CN 106806383 A CN106806383 A CN 106806383A CN 201510838955 A CN201510838955 A CN 201510838955A CN 106806383 A CN106806383 A CN 106806383A
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pachymaran
iron
preparation
iron complexes
precipitation
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彭代银
杜方平
陈卫东
俞年军
王妍妍
季兆洁
何瑞曦
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Anhui University of Traditional Chinese Medicine AHUTCM
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Anhui University of Traditional Chinese Medicine AHUTCM
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/24—Heavy metals; Compounds thereof
    • A61K33/26—Iron; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/70—Carbohydrates; Sugars; Derivatives thereof
    • A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/12—Carboxylic acids; Salts or anhydrides thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • Animal Behavior & Ethology (AREA)
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Abstract

The present invention relates to a kind of preparation method of pachymaran iron complexes, the content of iron is 4-6%, and the content of pachymaran is 40-65%, and the solubility at 25 DEG C in every 100mL water is 8-10g, and its preparation method is：Pachymaran and complexing agent are dissolved in distilled water, and the aqueous solution of ferric iron compound, pachymaran and complexing agent, FeCl are added dropwise afterwards3Mass ratio be 2:1:3, reaction is washed with ethanol and obtains pachymaran iron complexes after terminating, and the primary raw material of this method is by the use of the Poria cocos as integration of drinking and medicinal herbs, the dissolving out capability and stability of product are preferable, and abundance, stable preparation process, it is new iron deficiency agent there is provided new selection.

Description

A kind of preparation method of pachymaran iron complexes
Technical field
The invention belongs to polysaccharide compound technical field, particularly a kind of preparation method of pachymaran iron complexes.
Background technology
Iron is the essential trace element in human body, played an important role during body metabolism, when internal asiderosis, iron deficiency or hypoferric anemia occurs, though the iron content in molysite is very high, as iron supplementary, side effect is big, formulation chemist stability is poor, and the research to iron supplementary both at home and abroad shows, with the polyferose that polysaccharide and high price iron are generated（Polysaccharide Ion Complex, PIC）It is good with Small side effects, conformability stabilization, solubility as iron supplementary, the advantages of iron-holder is high, and part polysaccharide has complicated and diversified bioactivity and physiological function, compared with molysite, polyferose is more easy to be absorbed by organisms, both improve hematopoiesis function, also improve Ferritin Levels.
Poria cocos is On Polyporaceae Poria cocos Poria cocos (Schw.) dry sclerotia of Wolf, with clearing damp and promoting diuresis, strengthening the spleen and stomach, the effects such as antitoxic heart-soothing and sedative, the pachymaran extracted from Poria cocos is the main component of Poria cocos, account for the 70% ~ 92% of sclerotium, pachymaran can strengthen immunity of organisms, and with the effect such as anti-oxidant, antibacterium, antiviral, antitumor, the method is that, with pachymaran as raw material, by the way that heat is obtained pachymaran iron complexes altogether with ferric trichloride, raw material sources enrich, stable preparation process, for new iron deficiency agent provides new selection.
The content of the invention
The problem to be solved in the present invention is to provide a kind of pachymaran iron complexes, and new raw material is provided to produce new iron-deficient iron supplementary.
The present invention solves above-mentioned technical problem with following technical scheme：
A kind of pachymaran iron complexes, the content of iron is 4-6%, and the content of pachymaran is 40-65%, and the solubility at 25 DEG C in every 100mL water is 8-10g.
The preparation method of pachymaran iron complexes is：Pachymaran and complexing agent are dissolved in distilled water, and the aqueous solution of ferric iron compound is added dropwise afterwards, and pachymaran is 2 with the mass ratio of complexing agent, ferric iron compound:1:3, reaction is washed with ethanol after terminating and obtains pachymaran iron complexes.
The specific method of the preparation of pachymaran is：Poria cocos after drying is crossed into 60 mesh sieves and obtains Poria cocos meal, respectively with ether, acetone in cable type extractor according backflow degreasing 4 hours, residue is 1 according to volume ratio:15 add water 80 DEG C soaks 4h, filtered through gauze collects filtrate, and residual residue is soaked 4h and extracted 2 times at 80 DEG C again, merging filtrate, it is 6 that filtrate is neutralized to pH with 10% acetic acid, after neutralization, it is concentrated under reduced pressure, supernatant adds ethanol to determining alcohol 80% overnight to collect precipitation afterwards again, precipitation is washed 2 times with absolute ethyl alcohol, acetone, ether successively with after distilled water cyclic washing desalination, after vacuum drying, weigh, obtain final product pachymaran.
Complexing agent is sodium alginate or trisodium citrate or sodium tartrate.
Ferric iron compound is ferric trichloride.
Addition mass ratio is 10% aqueous sodium carbonate 2mL；It is 9 to adjust pH with the NaOH that mass ratio is 20%；Water bath heating temperature is 80 DEG C, and mixing time is 1.5h；While hot in 4000r/min centrifugations 3min；Take upper strata dark red solution, concentration is added for red-brown precipitation material occurs in 80% ethanol, stand overnight to the completely rear centrifugation of precipitation, precipitation obtains amorphous brown powder Thick many candies iron after drying, above-mentioned dry Thick many candies iron is taken, with concentration for 80% ethanol dissolves, slow-speed of revolution centrifugation is then carried out, gained precipitates low temperature drying, obtains purified polysaccharide iron.
, by the use of the Poria cocos as integration of drinking and medicinal herbs, the dissolving out capability and stability of product are preferable, and abundance, stable preparation process, for new iron deficiency agent provides new selection for the primary raw material of this method.
The advantage of the invention is that：
（1）The pachymaran iron Small side effects of present invention generation, conformability stabilization, solubility are good, and iron-holder is high；
（2）Compared with molysite, pachymaran iron is more easy to be absorbed by organisms, and both improves hematopoiesis function, also improves Ferritin Levels；
（3）Preparation process is simple, Poria cocos material source enriches, for new iron supplementary provides new selection.
Specific embodiment
The present invention is further illustrated below by way of specific embodiment, is not construed as limiting the invention in any form.
Embodiment 1 Prepare pachymaran iron complexes
Pachymaran 2.000g is weighed in the conical flask of 250mL, water dissolves are distilled with 80mL, add 1.000g sodium alginates, stirred and evenly mixed, add concentration for 10% aqueous sodium carbonate 2mL, the FeCl that concentration is 2mol/L is slowly added dropwise afterwards3 Solution 6mL,It is 9 to adjust pH with the NaOH that concentration is 20%,After 80 DEG C of stirred in water bath 1.5h,While hot in 4000r/min centrifugations 3min,Take upper strata dark red solution,Concentration is added for red-brown precipitation material occurs in 80% ethanol,Stand overnight to the completely rear centrifugation of precipitation,Precipitation obtains amorphous brown powder Thick many candies iron after drying,Take above-mentioned dry Thick many candies iron,With concentration for 80% ethanol dissolves,Then slow-speed of revolution centrifugation is carried out,Gained precipitates low temperature drying,Obtain purified polysaccharide iron complexes about 0.8g,Phend-sulphuric acid determines polyoses content about 58% in pachymaran compound,The content of iron is about 5.9% in phenanthroline determined by ultraviolet spectrophotometry compound,Compound is 8.1g per the solubility in 100mL water at 25 DEG C.
Embodiment 2 Prepare pachymaran iron complexes
Pachymaran 2.000g is weighed in the conical flask of 250mL, water dissolves are distilled with 80mL, add 1.000g trisodium citrates, stirred and evenly mixed, add concentration for 10% aqueous sodium carbonate 2mL, the FeCl that concentration is 2mol/L is slowly added dropwise afterwards3 Solution 6mL, it is 9 to adjust pH with the NaOH that concentration is 20%, after 80 DEG C of stirred in water bath 1.5h, while hot in 4000r/min centrifugations 3min, take upper strata dark red solution, concentration is added for red-brown precipitation material occurs in 80% ethanol, is stood overnight to the complete rear centrifugation of precipitation, precipitation obtains amorphous brown powder Thick many candies iron after drying.Take above-mentioned dry Thick many candies iron, with concentration for 80% ethanol dissolves, then slow-speed of revolution centrifugation is carried out, gained precipitates low temperature drying, obtain purified polysaccharide iron complexes about 0.8g, phend-sulphuric acid determines polyoses content about 47% in pachymaran compound, and the content of iron is about 5.4% in phenanthroline determined by ultraviolet spectrophotometry compound, and compound is 8.9g per the solubility in 100mL water at 25 DEG C.
Embodiment 3 Prepare pachymaran iron complexes
Pachymaran 2.000g is weighed in the conical flask of 250mL, water dissolves are distilled with 80mL, add 1.000g sodium tartrates, stirred and evenly mixed, add concentration for 10% aqueous sodium carbonate 2mL, the FeCl that concentration is 2mol/L is slowly added dropwise afterwards3 Solution 6mL,It is 9 to adjust pH with the NaOH that concentration is 20%,After 80 DEG C of stirred in water bath 1.5h,While hot in 4000r/min centrifugations 3min,Take upper strata dark red solution,Concentration is added for red-brown precipitation material occurs in 80% ethanol,Stand overnight to the completely rear centrifugation of precipitation,Precipitation obtains amorphous brown powder Thick many candies iron after drying,Take above-mentioned dry Thick many candies iron,With concentration for 80% ethanol dissolves,Then slow-speed of revolution centrifugation is carried out,Gained precipitates low temperature drying,Obtain purified polysaccharide iron complexes about 0.8g,Phend-sulphuric acid determines polyoses content about 52% in pachymaran compound,The content of iron is about 4.1% in phenanthroline determined by ultraviolet spectrophotometry compound,Compound is 9.8g per the solubility in 100mL water at 25 DEG C.
Embodiment 4 Prepare pachymaran
Weigh and 60 mesh sieve Poria cocos meal 1kg are crossed after drying, respectively with ether, acetone in cable type extractor according backflow degreasing 4 hours, residue is 1 according to volume ratio:15 add water 80 DEG C soaks 4h, filtered through gauze collects filtrate, and residual residue is soaked 4h and extracted 2 times at 80 DEG C again, merging filtrate, it is 6 that filtrate is neutralized to pH with 10% acetic acid, after neutralization, it is concentrated under reduced pressure, supernatant adds ethanol to determining alcohol 80% overnight to collect precipitation afterwards again, precipitation is washed 2 times with absolute ethyl alcohol, acetone, ether successively with after distilled water cyclic washing desalination, after vacuum drying, weigh, obtain pachymaran 15g.

Claims (6)

1. a kind of pachymaran iron complexes, it is characterised in that the content of iron is 4-6%, and the content of pachymaran is 40-65%, per the solubility in 100mL water are 8-10g at 25 DEG C.
2. the preparation method of a kind of pachymaran iron complexes according to claim 1, it is characterised in that the specific method of the formation of pachymaran compound is：Pachymaran and complexing agent are dissolved in distilled water, and the aqueous solution of ferric iron compound is added dropwise afterwards, and pachymaran is 2 with the mass ratio of complexing agent, ferric iron compound:1:3, reaction is washed with ethanol after terminating and obtains pachymaran iron complexes.
3. the preparation method of a kind of pachymaran iron complexes according to claim 2, it is characterised in that the specific method of the preparation of described pachymaran is：Poria cocos after drying is crossed into 60 mesh sieves and obtains Poria cocos meal, respectively with ether, acetone in cable type extractor according backflow degreasing 4 hours, residue is 1 according to volume ratio:15 add water 80 DEG C soaks 4h, filtered through gauze collects filtrate, and residual residue is soaked 4h and extracted 2 times at 80 DEG C again, merging filtrate, it is 6 that filtrate is neutralized to pH with 10% acetic acid, after neutralization, it is concentrated under reduced pressure, supernatant adds ethanol to determining alcohol for 80% overnight collects precipitation afterwards again, precipitation is washed 2 times with absolute ethyl alcohol, acetone, ether successively with after distilled water cyclic washing desalination, after vacuum drying, weigh, obtain final product pachymaran.
4. the preparation method of a kind of pachymaran iron complexes according to claim 2, it is characterised in that complexing agent is sodium alginate or trisodium citrate or sodium tartrate.
5. the preparation method of a kind of pachymaran iron complexes according to claim 2, it is characterised in that ferric iron compound is ferric trichloride.
6. the preparation method of a kind of pachymaran iron complexes according to claim 2, it is characterised in that addition mass ratio is 10% aqueous sodium carbonate 2mL；It is 9 to adjust pH with the NaOH that mass ratio is 20%；Water bath heating temperature is 80 DEG C, and mixing time is 1.5h；3min is centrifuged in 4000r/min while hot；Take upper strata dark red solution, concentration is added for red-brown precipitation material occurs in 80% ethanol, stand overnight to the completely rear centrifugation of precipitation, precipitation obtains amorphous brown powder Thick many candies iron after drying, above-mentioned dry Thick many candies iron is taken, with concentration for 80% ethanol dissolves, slow-speed of revolution centrifugation is then carried out, gained precipitates low temperature drying, obtains purified polysaccharide iron.
CN201510838955.9A 2015-11-27 2015-11-27 A kind of preparation method of pachymaran iron complexes Pending CN106806383A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102198151A (en) * 2011-05-18 2011-09-28 天津中敖生物科技有限公司 Bulk pharmaceutical of swine astragalus polyferose and preparation method thereof
CN103330718A (en) * 2013-06-20 2013-10-02 广西大学 Preparation method of gynostemma pentaphyllum polysaccharide-iron complex

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102198151A (en) * 2011-05-18 2011-09-28 天津中敖生物科技有限公司 Bulk pharmaceutical of swine astragalus polyferose and preparation method thereof
CN103330718A (en) * 2013-06-20 2013-10-02 广西大学 Preparation method of gynostemma pentaphyllum polysaccharide-iron complex

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
崔颂英: "《药用大型真菌生产技术》", 30 September 2009 *

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