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Preparation method of oxalic acid hydroxylamine vanadium coordination compound crystalloid with bioactivity

A technology of hydroxylamine vanadium oxalate and biological activity is applied in the field of preparation of hydroxylamine vanadium oxalate complex crystals, which can solve the problems of large required dosage, low absorption and utilization rate, low fat solubility and the like, and achieves good antidiabetic activity, simple method, short time effect

Inactive Publication Date: 2012-11-28
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Inorganic vanadate has high toxicity, low fat solubility, low bioavailability, and large dosage, so its absorption and utilization rate in organisms is low, and a large amount of use has great toxic and side effects, thus affecting its use in medicine. Wide range of applications in the field

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Step 1: Dissolve 0.3561g of lithium hydroxide and 0.1587g of ammonium metavanadate in a 25ml container I filled with 15ml of water under constant stirring in an ice-water bath, and stir to dissolve them. Then add 0.2356g oxalic acid and 0.4677g hydroxylamine hydrochloride in turn, stir and dissolve, then add 1mol / l hydrochloric acid solution dropwise to adjust the pH value of the solution to 6.86 to obtain a light yellow-green clear solution.

[0014] In the second step, put 15ml of absolute ethanol in another 100ml container II, put the container I containing the reaction solution in the first step into container II, seal it, place it in a refrigerator at 4°C, and let it stand. After standing for 3 days, white needle-like crystals were precipitated at the bottom of the small beaker.

[0015] Step 3: Take out the crystals at the bottom of the beaker, wash them with deionized water three times, then wash them with absolute ethanol and ether three times in turn, and place...

Embodiment 2

[0018] Step 1: Dissolve 0.3661g of lithium hydroxide and 0.1687g of ammonium metavanadate in a 25ml container I filled with 15ml of water under constant stirring in an ice-water bath, and stir to dissolve them. Then add 0.2359g oxalic acid and 0.4687g hydroxylamine hydrochloride in turn, stir and dissolve, then add 1mol / l hydrochloric acid solution dropwise to adjust the pH value of the solution to 6.64 to obtain a light yellow-green clear solution.

[0019] In the second step, put 15ml of absolute ethanol in another 100ml container II, put the container I containing the reaction solution in the first step into container II, seal it, place it in a refrigerator at 4°C, and let it stand. After standing for 4 days, white needle-like crystals were precipitated at the bottom of the small beaker.

[0020] Step 3: Take out the crystals at the bottom of the beaker, wash them with deionized water three times, then wash them with absolute ethanol and ether three times in turn, and place...

Embodiment 3

[0023] Step 1: Dissolve 0.3581g of lithium hydroxide and 0.1589g of ammonium metavanadate in a 25ml container I filled with 15ml of water under constant stirring in an ice-water bath, and stir to dissolve them. Then add 0.2358g oxalic acid and 0.4678g hydroxylamine hydrochloride in turn, stir and dissolve, then add 1mol / l hydrochloric acid solution dropwise to adjust the pH value of the solution to 6.56 to obtain a light yellow-green clear solution.

[0024] In the second step, put 15ml of absolute ethanol in another 100ml container II, put the container I containing the reaction solution in the first step into container II, seal it, place it in a refrigerator at 4°C, and let it stand. After standing for 5 days, white needle-like crystals were precipitated at the bottom of the small beaker.

[0025] Step 3: Take out the crystals at the bottom of the beaker, wash them with deionized water three times, then wash them with absolute ethanol and ether three times in turn, and place...

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PUM

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Abstract

The invention discloses a preparation method of an oxalic acid hydroxylamine vanadium coordination compound crystalloid with bioactivity. By taking ammonium ion as external balance ion to be participated in the coordination compound, the method comprises the steps of: (1) stirring ammonium metavanadate, lithium hydroxide, oxalic acid, hydroxylamine hydrochloride and water to be dissolved in a container I under the condition of 0-4 DEG C, and adjusting the PH value of the solution by hydrochloride solution to obtain light yellowgreen cleaning solution; (2) adding absolute ethyl alcohol into another larger container II, putting the container I which is filled with reaction solution in the step (1) in to the container II, sealing the container II, putting the container II into a refrigerator, and stewing for 3-7 days, so that white acicular crystal is separated out of the bottom of the container I; and (3) withdrawing the crystal at the bottom of the container I, cleaning the crystal by deionized water at several times, cleaning the crystal by absolute ethyl alcohol and ethyl alcohol at several times respectively, putting the cleaned crystal into a drier to obtain the dried and cleaned crystalloid which is the oxalic acid hydroxylamine vanadium coordination compound crystalloid with the bioactivity. The bioactivity of the crystalloid obtained by the method is good. The preparation method is simple, easy to operate, and short in time.

Description

technical field [0001] The invention relates to a preparation method of crystals, in particular to a preparation method of biologically active hydroxylammonium oxalate vanadium complex crystals. Background technique [0002] Vanadium is an essential trace element in some animals, and may play a very important role in the metabolism of glucose. Studies have found that some complexes of inorganic vanadate and vanadium organic ligands have good insulin-like activity. A small number of vanadium compounds have been put into clinical trials. Inorganic vanadate has high toxicity, low fat solubility, low bioavailability, and large dosage, so its absorption and utilization rate in organisms is low, and a large amount of use has great toxic and side effects, thus affecting its use in medicine. wide range of applications in the field. In view of this, it is very important to increase the bioavailability of vanadium compounds and reduce their toxicity. A common method to solve these p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/08C30B29/54
Inventor 单永奎张其颖金忠敏杨琼范鑫张恒强
Owner EAST CHINA NORMAL UNIV
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