CN101328222B - Liquorice polyose metal complexes and preparation thereof - Google Patents
Liquorice polyose metal complexes and preparation thereof Download PDFInfo
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Abstract
The invention relates to a chemical product and a preparation method thereof, namely a glycyrrhiza polysaccharide metal complex and a method for preparing glycyrrhiza polysaccharide. Various metallic cations have the function of medical care, but the metallic cations can only be utilized by the human body when combined with various carriers; however, the prior carrier materials mostly have no nutrient value and a part of the carrier materials can not be directly utilized. The method extracts the glycyrrhiza polysaccharide with medical care function from the prior medicinal material liquorice through a plurality of experimental researches, and synthesizes various glycyrrhiza polysaccharide metal complexes through the glycyrrhiza polysaccharide and metallic cation compounds. As proved by the researches, the complex not only has respective advantages of the glycyrrhiza polysaccharide and metallic ions but also has excellent functions of supraposition and reinforcement, can be widely used in the manufacturing industries of various foodstuffs, medicines and health products, can obviously improve the medical care level of products, shorten the product volume, and reduce the toxic side effect, and has wide application prospect.
Description
Affiliated technical field
The present invention relates to the manufacture method of a kind of chemical products and this product, i.e. liquorice polyose metal complexes and preparation method thereof.
Background technology
Metallic element plays an important role in whole life system, and known 25 kinds of elements are essential by life entity.The feature of metal maximum is exactly to lose electronics to become positively charged ion, be present in the biological fluid is various forms of metal ions, they can produce various interactions with biomolecules, thereby bear various functions in vivo, as active centre of transfer transport, oxygen carrier, enzyme etc., metal ion must with how to combine with carrier substance, could be utilized by the people, the then many no medical care effects of its carrier, what have can't directly utilize.For example: be used for the zinc sulfate of zinc supplementation, the nutritive value of its acid group is just imprecise, need get rid of by the metabolic process of human body.Be used to mend the Sodium Selenite of selenium, can't directly take, and need to become grain, vegetables or meat, eggs and milk based food and play a role again by complicated biotransformation.Therefore, people wish metallic cation and have nutrition, material medicinal, health-care effect combines, thereby reinforced effects is simplified the process of utilizing.In recent years it is found that, the intravital many saccharide compounds of people can interact with metal ion and produce different biological functions, suppress various oxyradicals such as hydroxyl radical free radical, ultra-oxygen anion free radical and lipid free radical as polysaccharide and metal ion interaction energy, compound and suppress the breeding of bacterium and tumour cell with DNA, play antibacterial bacteriostatic, suppress the effect that tumour cell generates.Can foretell thus,, should produce beyond thought pharmaceutical use or health care value if can get up polysaccharide and melts combine.
Summary of the invention
The objective of the invention is licorice polysaccharide and melts combine, obtain liquorice polyose metal complexes, and propose the preparation method of liquorice polyose metal complexes.
Analyze by experiment, obtain liquorice polyose metal complexes, the title complex that comprises all metallic cations such as calcium, iron, zinc, selenium, tungsten, magnesium, nickel, copper, cobalt, titanium and licorice polysaccharide, the diffuse reflectance infrared spectroscopy peak data of its expression constructional feature is 3195.1-3660.76 (OH), 2920.97-2937.48 (CH2-), 1632.98-1643.02 (C=O), 1127.16-1151.79 (C-O-C), 1025.60-1081.19 (C-O-H), 1082.92cm wherein
-1, 1020.96cm
-1Be pyranose characteristic peak, 928.73,851.49cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
The preparation method of above-mentioned liquorice polyose metal derivative is: licorice polysaccharide dissolving back is added the metallic cation compound get the liquorice polyose metal mixed solution, reaction solution PH=6-7, after filtration filtrate, again dialyzate concentrate, alcohol is analysed, precipitate, washing, drying, obtains the polyose metal material.
The preparation method of described liquorice polyose metal complexes is: the extracting liquorice polysaccharide is dissolved in water, and adds the metal ion solution of 1mol/L.To between the 6-7,2-4 hours postcooling of low-grade fever reaction, filtration concentrate alcohol with filtrate and analyse with the adjusting PH with base value, the brown material be crude product.Again with dissolving crude product, dialysis (dialysis tubing XH420, the scope of damming 8000--10000) is purified, with dialyzate concentrate, alcohol is analysed, precipitate, washing, drying, and the liquorice polyose metal material of certain color must be arranged.
The preparation method of above-mentioned liquorice polyose metal complexes comprises the reparation technology of licorice polysaccharide, the reparation technology of licorice polysaccharide comprises that Crude polysaccharides extracts and polysaccharide purification two-stage process: its raw sugar extraction process is: raw material pulverizing, add that water stirs, the heating extraction, with the extracting solution concentrating under reduced pressure, add ethanol sedimentation, leave standstill, suction filtration, with dehydrated alcohol, ether washing, the dry Crude polysaccharides that gets of decompress filter; Its purifying technique is: Crude polysaccharides is dissolved in water, puts into dialysis removal of impurities in the dialysis tubing (dialysis tubing XH420, the scope of damming 8000--10000), with solution concentration, alcohol is analysed, and decompress filter is respectively with ethanol, the dry licorice polysaccharide that gets of ether washing.
Said liquorice polyose metal complexes comprises licorice polysaccharide tungsten, and its diffuse reflectance infrared spectroscopy peak data is 3660.76-3416.19 (OH), 2937.48 (CH
2-), 1638.43 (C=O), 1139.39 (C-O-C), 1045.12 (C-O-H), 951.29-893.07,850.35-804.57cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
Said liquorice polyose metal complexes comprises licorice polysaccharide selenium, and its diffuse reflectance infrared spectroscopy peak data is that 3382.23 (OH), 2929.85 (CH2-), 1643.02 (-C=O), 1151.31 (-C-O-C), 1080.55-1028.13 (C-O-H), 765.80-707.48cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
Said liquorice polyose metal complexes comprises licorice polysaccharide iron, and its diffuse reflectance infrared spectroscopy peak data is 3381.09 (OH), 2930.85 (CH
2-), 1641.88 (C=O), 1150.82 (C-O-C), 1081.19 (C-O-H), 760.84-850.88cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
Said liquorice polyose metal complexes comprises licorice polysaccharide calcium, and its diffuse reflectance infrared spectroscopy peak data is that 3385.55 (OH), 2930.16 (CH2-), 1641.66 (-C=O), 1151.79 (-C-O-C), 1077.23-1026.24 (C-O-H), 855.45-763.50cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
Said liquorice polyose metal complexes comprises the licorice polysaccharide titanium, and its diffuse reflectance infrared spectroscopy peak data is that 3195.10 (OH), 2920.97 (CH2-), 1632.98 (-C=O), 1127.16 (-C-O-C), 1077.23-1045.97 (C-O-H), 780.20-755.76cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
Said liquorice polyose metal complexes comprises licorice polysaccharide zinc, its diffuse reflectance infrared spectroscopy peak data is 3380.76 (OH), 2926.08 (-CH2-), 1639.55 (-C=O), 1151.68 (-C-O-C), 1081.09-1027.39 (C-O-H), 934.65-863.73,765.04-708.62cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
The liquorice polyose metal complexes that adopts technique scheme to produce, this title complex has not only kept licorice polysaccharide and metal ion advantage separately, and has an outstanding additive effect, can be widely used in the production of varieties of food items, medicine, healthcare products, can obviously improve the health care level of product, dwindle small product size, reduce toxic side effect, have broad application prospects.
Description of drawings
Fig. 1 is the infrared spectrogram of licorice polysaccharide;
Fig. 2 is the infrared spectrogram of licorice polysaccharide tungsten;
Fig. 3 is the infrared spectrogram of licorice polysaccharide selenium;
Fig. 4 is the infrared spectrogram of licorice polysaccharide iron;
Fig. 5 is the infrared spectrogram of licorice polysaccharide calcium;
Fig. 6 is the infrared spectrogram of licorice polysaccharide zinc;
Fig. 7 is the technological process of production figure of liquorice polyose metal.
Embodiment
The present invention is by a large amount of experimental analyses, grasped the constructional feature of liquorice polyose metal complexes, on this basis, again the pharmaceutical use and the health-care effect of liquorice polyose metal complexes are inquired into, proved that this material has no side effect to human body, and can obviously improve people's blood viscosity, reduce thrombotic speed and probability, at anti-tumor aspect positive curative effect is arranged also, effects such as its medicine and healthcare products are better than polysaccharide, thereby have important potentiality to be exploited.Introduce five kinds of embodiment below:
First kind of embodiment: the extraction method of purification of licorice polysaccharide.
1. Radix Glycyrrhizae raw sugar extraction process: with raw material pulverizing, add the water stirring heating, extracted 2.5-3.5 hours down at 70-80 ℃, 3 times repeatedly, united extraction liquid, evaporation concentration add the ethanol sedimentation of 2-4 times of concentrated solution volumes to 50mL, left standstill 20-28 hours, suction filtration is washed 2 times with dehydrated alcohol, and ether is washed 2 times, decompress filter gets Crude polysaccharides, places moisture eliminator dry.
2. the purifying technique of licorice polysaccharide: Crude polysaccharides is dissolved in water, put into dialysis tubing (dialysis tubing XH420, the scope of damming 8000--10000) in, dialysed 68-75 hours, remove small molecular weight impurities such as oligose, with solution concentration, alcohol is analysed, decompress filter is respectively with ethanol, the dry Radix Glycyrrhizae holosaccharide that gets of ether washing.
The physicochemical character of products obtained therefrom: the licorice polysaccharide pale powder, do not have smell, tasteless, soluble in water, its aqueous solution is the red-brown clear solution, is neutral.Be insoluble to organic solvents such as anhydrous methanol, ethanol, ether.
The structure of product: by licorice polysaccharide infrared spectrogram shown in Figure 1, its characteristic peak data are as can be known: 3362.43 (OH), 2928.57 (CH2-), 1639.01 (-C=O), 1151.56 (-C-O-C), 1079.75-1026.52 (C-O-H), 862.26cm wherein
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
Second kind of embodiment: the preparation method of licorice polysaccharide tungsten.
The extracting liquorice polysaccharide is dissolved in water, and adds the sodium tungstate solution of 1mol/L.To between the 6-7,2-4 hours postcooling of low-grade fever reaction, filtration concentrate alcohol with filtrate and analyse with the adjusting PH with base value, light material be crude product.Again with dissolving crude product, dialysis (dialysis tubing XH420, the scope of damming 8000--10000) is purified, with dialyzate concentrate, alcohol is analysed, precipitate, washing, drying, light material be licorice polysaccharide tungsten.
The structure of product: by licorice polysaccharide tungsten infrared spectrogram shown in Figure 2, the diffuse reflectance infrared spectroscopy peak data of licorice polysaccharide tungsten is as can be known: 3660.76-3416.19 (OH), 2937.48 (CH
2-), 1638.43 (C=O), 1139.39 (C-O-C), 1045.12 (C-O-H), 951.29-893.07,850.35-804.57cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
The third embodiment: the preparation method of licorice polysaccharide selenium.
The extracting liquorice polysaccharide is dissolved in water, and adds the SeSO of 1mol/L
3Solution.To between the 6-7,2-4 hours postcooling of low-grade fever reaction, filtration concentrate alcohol with filtrate and analyse with the adjusting PH with base value, light material be crude product.Again with dissolving crude product, dialyse (dialysis tubing XH420, the scope of damming 8000--10000) purifies, with dialyzate concentrate, alcohol is analysed, precipitate, washing, drying, light material be licorice polysaccharide selenium.
The structure of product: by licorice polysaccharide selenium ruby external spectrum figure shown in Figure 3, the diffuse reflectance infrared spectroscopy peak data of licorice polysaccharide iron is as can be known: 3382.23 (OH), 2929.85 (-CH2-), 1643.02 (-C=O), 1151.31 (-C-O-C), 1080.55-1028.13 (C-O-H), 765.80-707.48cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
The 4th kind of embodiment: the preparation method of licorice polysaccharide iron.
The extracting liquorice polysaccharide is dissolved in water, and adds the FeCl of 1mol/L
2Solution.To between the 6-7, the low-grade fever reaction is after 2-4 hours with the adjusting PH with base value of 0.5mol/L, cooling, filters, filtrate is concentrated alcohol analyses, slightly the material of color be crude product.Again with dissolving crude product, dialyse (dialysis tubing XH420, the scope of damming 8000--10000) purifies, will dialyse concentrate, alcohol is analysed, precipitate, washing, drying, must be licorice polysaccharide iron by the reddish-brown material.
The physicochemical character of products obtained therefrom: licorice polysaccharide iron is the reddish-brown powder, do not have smell, tasteless, soluble in water, its aqueous solution is reddish brown red clear solution, is neutral.Be insoluble to organic solvents such as anhydrous methanol, ethanol, ether.
The structure of product: by licorice polysaccharide iron oxide red external spectrum figure shown in Figure 4, the diffuse reflectance infrared spectroscopy peak data of licorice polysaccharide iron is as can be known: 3381.09 (OH), 2930.85 (CH
2-), 1641.88 (C=O), 1150.82 (C-O-C), 1081.19 (C-O-H), 760.84-850.88cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
The 5th kind of embodiment: sum up liquorice polyose metal calcium, iron, selenium, tungsten, zinc, magnesium, nickel, copper, cobalt, etc. preparation method and constructional feature, obtain the general preparation method and the overall structures of liquorice polyose metal.
The synthetic general formula that Fig. 7 introduced has been represented the general preparation method of liquorice polyose metal, comprises licorice polysaccharide dissolving, the purification that mixes, filters, dialyses with metal salt solution, reconcentration, alcohol are analysed, precipitate, drying, can obtain the liquorice polyose metal derivative.Concrete grammar is:
The extracting liquorice polysaccharide is dissolved in water, and adds the metal ion solution of 1mol/L.To between the 6-7,2-4 hours postcooling of low-grade fever reaction, filtration concentrate alcohol with filtrate and analyse with the adjusting PH with base value, light material be crude product.Again with dissolving crude product, dialysis (dialysis tubing XH420, the scope of damming 8000--10000) is purified, with dialyzate concentrate, alcohol is analysed, precipitate, washing, drying, obtains the liquorice polyose metal material of certain color.
The constructional feature of liquorice polyose metal: according to infrared spectrograms such as liquorice polyose metal calcium, iron, selenium, tungsten, zinc, magnesium, nickel, copper, cobalts, the infrared spectrogram of liquorice polyose metal is summarized in summary, its characteristic peak data are: 3195.1-3660.76 (OH), 2920.97-2937.48 (CH2-), 1632.98-1643.02 (C=O), 1127.16-1151.79 (C-O-C), 1025.60-1081.19 (C-O-H), 1082.92cm wherein
-1, 1020.96cm
-1Be pyranose characteristic peak, 928.73,851.49cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
The experiment overview:
The medical care effect of polysaccharide and metallic element confirms by a large amount of experiments and practical application, can infer licorice polysaccharide fully and metal complexes has value medical health care according to existing data.However, in order further to understand the special role for human body of liquorice polyose metal complexes, and distinctive mechanism of action, since 2005, we are according to the index of recommending in " DRIs " of Chinese Soclety of Nutrition's establishment, the nutrition feature of licorice polysaccharide iron, licorice polysaccharide zinc, licorice polysaccharide selenium, licorice polysaccharide calcium has been carried out experimentation on animals and the crowd observes, the medical care effect of liquorice polyose metal derivative has been carried out preliminary discussion.The oxidation-resistance of finding liquorice polyose metal obviously is better than licorice polysaccharide and multiple other metal ion supplement, proved that polysaccharide and metal interaction are more more remarkable to the influence that human body produces than single polysaccharide or multiple metallic salt material, illustrate that liquorice polyose metal complexes has not only kept licorice polysaccharide and the original effect of various metallic cation, and produced significant strengthening effect, show that produce effects is fast, strong drug action, dosage are little, be convenient to processing, be convenient to transportation, special advantages such as be convenient to take, and do not find any toxic side effect.
Discover that Polyferose, polysaccharide calcium and polysaccharide zinc all exist with solvable state in the pH=3-12 scope, promptly solubleness is very big, and this explanation Polyferose, polysaccharide calcium and polysaccharide zinc have bioavailability preferably.The control of metal content was relatively easy when also explanation prepared liquorice polyose metal simultaneously, this point, for having special meaning with an amount of absorption of guaranteeing metallic element, for liquorice polyose metal becomes supplement, particularly iron, zinc, the selenium of body trace element, the supplement of calcium provide condition.
Claims (7)
1. the preparation method of a liquorice polyose metal complexes, it is characterized in that: produce licorice polysaccharide earlier, comprise that Crude polysaccharides extracts and polysaccharide purification two-stage process: Radix Glycyrrhizae Crude polysaccharides extraction process: with raw material pulverizing, add the water stirring heating, extracted 2.5-3.5 hour down at 70-80 ℃, 3 times repeatedly, united extraction liquid, evaporation concentration add concentrated solution volume 2-4 ethanol sedimentation doubly to 50mL, left standstill 20-28 hour, suction filtration is washed 2 times with dehydrated alcohol, and ether is washed 2 times, decompress filter gets Crude polysaccharides, places moisture eliminator dry; The purifying technique of licorice polysaccharide: Crude polysaccharides is dissolved in water, puts into the XH420 dialysis tubing, the scope of damming 8000-10000, dialysed 68-75 hour, and removed small molecular weight impurities such as oligose, solution concentration, alcohol is analysed, and decompress filter is respectively with ethanol, the dry Radix Glycyrrhizae holosaccharide that gets of ether washing; The extracting liquorice polysaccharide is dissolved in water again, the metal ion solution that adds 1mol/L, here said metal ion is a kind of in tungsten ion, plasma selenium, iron ion, calcium ion, titanium ion, the zine ion, with the adjusting PH with base value between the 6-7,2-4 hour postcooling of low-grade fever reaction, filtration, filtrate is concentrated alcohol analyses, get light material and be crude product, again with dissolving crude product, again with the XH420 dialysis tubing, dialysis is purified under the condition of the scope of damming 8000-10000, with dialyzate concentrate, alcohol is analysed, precipitate, washing, drying, and the liquorice polyose metal material of certain color must be arranged.
2. the preparation method of liquorice polyose metal complexes according to claim 1, it is characterized in that: said liquorice polyose metal complexes comprises licorice polysaccharide tungsten, its diffuse reflectance infrared spectroscopy peak data is-OH:3660.76-3416.19-CH
2-: 2937.48 ,-C=O:1638.43 ,-C-O-C:1139.39 ,-C-O-H:1045.12,951.29-893.07,850.35-804.57cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
3. the preparation method of liquorice polyose metal complexes according to claim 1, it is characterized in that: said liquorice polyose metal derivative comprises licorice polysaccharide selenium, its diffuse reflectance infrared spectroscopy peak data is-OH:3382.23-CH
2-: 2929.85 ,-C=O:1643.02 ,-C-O-C:1151.31 ,-C-O-H:1080.55-1028.13,765.80-707.48cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
4. the preparation method of liquorice polyose metal complexes according to claim 1, it is characterized in that: said liquorice polyose metal complexes comprises licorice polysaccharide iron, its diffuse reflectance infrared spectroscopy peak data is-OH:3381.09-CH
2-2930.85 ,-C=O 1641.88 ,-C-O-C:1150.82 ,-C-O-H:1081.19,760.84-850.88cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
5. the preparation method of liquorice polyose metal complexes according to claim 1, it is characterized in that: said liquorice polyose metal complexes comprises licorice polysaccharide calcium, its diffuse reflectance infrared spectroscopy peak data is-OH:3385.55-CH
2-: 2930.16 ,-C=O:1641.66 ,-C-O-C:1151.79 ,-C-O-H:1077.23-1026.24,855.45-763.50cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
6. the preparation method of liquorice polyose metal complexes according to claim 1, it is characterized in that: said liquorice polyose metal derivative comprises the licorice polysaccharide titanium, its diffuse reflectance infrared spectroscopy peak data is-OH:3195.10-CH
2-: 2920.97 ,-C=O:1632.98 ,-C-O-C:1127.16 ,-C-O-H:1077.23-1045.97,780.20-755.76cm
-1Near absorption peak is the charateristic avsorption band of α-pyranose glycosidic bond.
7. the preparation method of liquorice polyose metal complexes according to claim 1, it is characterized in that: said liquorice polyose metal complexes comprises licorice polysaccharide zinc, its diffuse reflectance infrared spectroscopy peak data is-OH:3380.76-CH
2-: 2926.08 ,-C=O:1639.55 ,-C-O-C:1151.68 ,-C-O-H:1081.09-1027.39,934.65-863.73,765.04-708.62cm
-1Near absorption peak is respectively the charateristic avsorption band of β-pyranose and α-pyranose glycosidic bond.
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