Preparation method of biological active hydroxylamine oxalate vanadium complex crystal

A technology of vanadium oxalate vanadium and biological activity, which is applied in the field of preparation of vanadium oxalate complex crystals, can solve the problems of large dosage, low absorption utilization rate, toxic and side effects, etc., achieve good anti-diabetic activity, simple method, and easy The effect of the operation

Inactive Publication Date: 2014-11-05
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

[0014] The first step is to dissolve 0.3961g of rubidium carbonate and 0.1017g of ammonium metavanadate in a 25ml beaker filled with 10ml of water, stir to dissolve them, then add 0.1551g of oxalic acid, and finally add 0.1677g of hydroxylamine hydrochloride under ice bath conditions , after stirring and dissolving, add 0.5 mol / l hydrochloric acid solution dropwise to adjust the pH value of the solution to 6.85 to obtain a light yellow clear solution.

[0015] In the second step, put 5ml of absolute ethanol in another 100ml container II, put the container I containing the reaction solution in the first step into the container II, seal it, place it in a refrigerator at 4°C, and let it stand. After standing for 3 days, colorless flaky crystals precipitated out at the bottom of the small beaker.

[0016] 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 pla...

Embodiment 2

[0019] The first step is to dissolve 0.3985g of rubidium carbonate and 0.1056g of ammonium metavanadate in a 25ml beaker filled with 12ml of water, stir to dissolve them, then add 0.1531g of oxalic acid, and finally add 0.1654g of hydroxylamine hydrochloride under ice bath conditions , after stirring and dissolving, add 0.8 mol / l hydrochloric acid solution dropwise to adjust the pH value of the solution to 6.77 to obtain a light yellow clear solution.

[0020] In the second step, put 7ml 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 3°C, and let it stand. After standing for 2 days, colorless flaky crystals precipitated out at the bottom of the small beaker.

[0021] Step 3: Take out the crystals at the bottom of the beaker, wash them three times with deionized water, then wash them with absolute ethanol and ether three times in turn, and place t...

Embodiment 3

[0024] The first step is to dissolve 0.3988g rubidium carbonate and 0.1078g ammonium metavanadate in a 25ml beaker filled with 11ml water, stir to dissolve them, then add 0.1588g oxalic acid, and finally add 0.1658g hydroxylamine hydrochloride under ice bath conditions After stirring and dissolving, add 0.7 mol / l hydrochloric acid solution dropwise to adjust the pH value of the solution to 6.45 to obtain a light yellow clear solution.

[0025] In the second step, put 6ml of absolute ethanol in another 100ml container II, put the container I containing the reaction solution in the first step into the container II, seal it, place it in a refrigerator at 0°C, and let it stand. After standing for 3 days, colorless flaky crystals precipitated out at the bottom of the small beaker.

[0026] Step 3: Take out the crystals at the bottom of the beaker, wash them three times with deionized water, then wash them with absolute ethanol and ether three times in turn, and place them in a desi...

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Abstract

The invention discloses a preparation method of a biological active hydroxylamine oxalate vanadium complex crystal, and the method uses Rb <+ >ions as external balance ions for participating into the complex, and comprises the following steps: 1, at 0-4 DEG C, rubidium carbonate, ammonium metavanadate, oxalic acid, hydroxylamine hydrochloride and water are stirred and dissolved in a container I, the pH value of the solution is adjusted by a hydrochloric acid solution to obtain a pale yellow clear solution; 2, anhydrous alcohol is added into another container II, the container I filled with the reaction liquid in the step 1 is put in the container II, the container II is sealed, and placed in a refrigerator for standing for 2 to 4 days, and a colorless flaky crystal is precipitated on the container I bottom; and 3, the crystal precipitated on the container I bottom is taken out, washed with deionized water for a plurality of times, then is successively washed respectively with the anhydrous ethanol and ether for a plurality of times, and then is put in a dryer to obtain dry and pure crystal, namely the biological active hydroxylamine oxalate vanadium complex crystal. The obtained biological active hydroxylamine oxalate vanadium complex crystal is good in biological activity, and the preparation method is simple, easy in operation, 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 Applications(China)
IPC IPC(8): C07F9/00A61P3/10
Inventor 张其颖李秀彩
Owner EAST CHINA NORMAL UNIV
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