CN101433549A - Calcium oxalate crystallization inhibitor and uses thereof - Google Patents

Calcium oxalate crystallization inhibitor and uses thereof Download PDF

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CN101433549A
CN101433549A CNA2008102198882A CN200810219888A CN101433549A CN 101433549 A CN101433549 A CN 101433549A CN A2008102198882 A CNA2008102198882 A CN A2008102198882A CN 200810219888 A CN200810219888 A CN 200810219888A CN 101433549 A CN101433549 A CN 101433549A
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calcium oxalate
solution
moll
selenium
nanometer selenium
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CN101433549B (en
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白燕
梁敏思
郑文杰
周艳晖
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Jinan University
University of Jinan
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Abstract

The invention discloses calcium oxalate crystallization inhibitor and application thereof. The inhibitor is prepared by nano selenium which is obtained by mixed reaction of selenite solution and vitamin C solution according to certain proportion. Preferably, the selenite is sodium selenite or selenium dioxide, and the vitamin C is reduced vitamin C. The invention uses the nano selenium to prepare the calcium oxalate crystallization inhibitor for the first time; and the obtained inhibitor can effectively inhibit growth and gather of calcium oxalate, and can be used for preparing calculus inhibiting medicament of the calcium oxalate.

Description

A kind of calcium oxalate crystal inhibitor and application thereof
Technical field
The invention belongs to the preparation field of calculus inhibitor, be specifically related to a kind of with calcium oxalate crystal inhibitor and application thereof.
Background technology
Nanometer selenium (selenic Nano sol) is the minimum selenium-replenishing preparation of having found of acute toxicity.Aspect biological effect, the external removing hydroxy radical of nanometer selenium efficient is 5 times of inorganic selenium, is 2.5 times of organic selenium.Nanometer selenium is promptly demonstrating under low dosage very and is suppressing tumor and immunomodulating health-care effect, and the inorganic selenium of corresponding low dosage there is no effect, the health-care effect of the nanometer selenium sensitive characteristics that shows abnormality.Nanometer selenium is removed the same with inorganic selenium and organic selenium, has beyond the very high biologic activity, and it also has other characteristics that are different from both: 1, high bioactivity.Do the carrier of medicine or antibody with nanoparticle, can improve some drugs and see through natural or synthetical membrane structure, and be accumulated in small intestinal, make the bioavailability of medicine that remarkable improvement arranged.Present stage, achievement in research showed, compare with marker, nanometer selenium has biological effect efficiently.2, high security.Document announcement is arranged both at home and abroad, and nanometer selenium is the highest selenium preparation of safety, and it is 1/7～1/10 of a selenium marker to the toxicity of mice, is the minimum selenium preparation of known acute toxicity.One of reason that the acute toxicity of nanometer selenium is very low may be that nanometer selenium and organism glutathion inside reflection ratio are low and then the free-radical generating amount is low.3, high immune regulative: discover cell, body fluid, the nonspecific immunity function of nanometer selenium energy significant stimulation organism, thereby the diseases prevention and the resistance against diseases of raising body.Experimentation shows that nanometer selenium more is better than organic selenium in many aspects, demonstrates the efficient feature of low toxicity, and the biological effectiveness of nanometer selenium is just approved that health ministry approved nanometer selenium capsule is a health food.
In industry and medical field, the research of calcium oxalate crystals is very paid close attention to.In industrial aspect for example paper-making industry, sugar industry and beverage finishing sector etc., cause and consume more energy and more production time of waste because the formation of calcium oxalate crystals is slowed down the heat transmission.The process of association with pulp bleaching and sugaring for example, calcium oxalate scaling can be suspended in the water, perhaps forms hard deposit, accumulate on the surface of any material that contacts with water, this gathering can stop effective heat transfer, hinders fluid flow, causes corrosion and hiding antibacterial.Aspect medical, calcium oxalate stone is the main matter of calculus of urethra.The most stable Calcium oxalate (CaC2O4) monohydrate (COM) of thermodynamics is the most general in urinary system calculus and urine, accounts for calculus content 60%, and metastable calcium oxalate dihydrate (COD) takes second place, and three water calcium oxalates (COT) are that thermodynamics is least stable.Can make calcium oxalate crystals crystallize speed from its saturated solution slow down or reduce crystal formation material and promptly be called its inhibitor.Industry medical aspect, once reported the inhibitor of a lot of calcium oxalates, for example polyeletrolyte (Akyol, Emel; Oener, Mualla.Inhibition of calcium oxalate monohydrate crystal growth usingpolyelectrolytes.Journal of Crystal Growth (2007), 307 (1), 137-144.), citrate (Wang, Lijun; Zhang, Wei; Qiu, S.Roger; Zachowicz, William J.; Guan, Xiangying; Tang, Ruikang; Hoyer, John R.; De Yoreo, James J.; Nancollas; GeorgeH.Inhibition of calcium oxalate monohydrate crystallization by the combination ofcitrate and osteopontin.Journal of Crystal Growth (2006); 291 (1); 160-165.), polysaccharide (Deng Suiping; Wu Xiumei, Ou Yangjianming. Sargassum Eucheuma striatum polysaccharide suppresses the research of urinary calculi oxalic salt calcium crystal growth. SCI, (2006); 8 (1), 595-598.) etc.People such as Ah's Brahms have applied for the patent (CN1503668A) of relevant use rare earth compound prevention renal calculus.Also do not report the inhibitor of relevant selenium so far as calcium oxalate.
The preparation that above-mentioned various calculus inhibitor has is purified complicated, and the composition complexity that has may cause certain side effect to human body, nanometer selenium is applied as the calculus inhibitor possesses the prospect that overcomes aforesaid drawbacks.
Summary of the invention
For overcoming above-mentioned problems of the prior art and deficiency, the purpose of this invention is to provide a kind of calcium oxalate crystal inhibitor and application thereof of mainly making by nanometer selenium.
For realizing purpose of the present invention, the technical solution used in the present invention is as follows: a kind of calcium oxalate crystal inhibitor is characterized in that: be to be made by nanometer selenium.
Described nanometer selenium is by industry selenate solution and vitamin c solution hybrid reaction and obtain.
To better implement the present invention:
Ascorbic concentration is 4 * 10 in the described vitamin c solution -4～4 * 10 -2MolL -1, the concentration of the selenite in the described selenite solution is 2 * 10 -4～2 * 10 -2MolL -1The volumetric usage of described vitamin c solution and described selenite solution is than preferred 1: 0.5～2.
Described ascorbic concentration more preferably 4 * 10 -3MolL -1The concentration of described selenite more preferably 2 * 10 -3MolL -1
Described vitamin c solution compared more preferably 1: 1 with the volumetric usage of selenite solution.
Preferred sodium selenite of described selenite or selenium dioxide.
Described vitamin C preferably refers to the reduced form vitamin C.
The present invention has further studied the depression effect of above-mentioned calcium oxalate crystal inhibitor for the calcium oxalate crystal growth, result of study shows, inhibitor of the present invention can effectively suppress the calcium oxalate growth and assemble, thereby can be used in preparation calcium oxalate stone suppressive drug fully.
Beneficial effect of the present invention is as follows: the present invention is applied as nanometer selenium the calcium oxalate crystal inhibitor first, and its preparation technology is simple.Products obtained therefrom not only can be used for preparing medical fields such as calculus inhibitor, is relating to the also application prospects of industrial circle that suppresses calcium oxalate crystal.
Description of drawings
Fig. 1 is observed calcium oxalate crystals growth control figure under scanning electron microscope (SEM),
Wherein, a. does not have the interpolation inhibitor; B. add 2 * 10 -5MolL -1Nanometer selenium; C. add 2 * 10 -5MolL -1SeO 2
Fig. 2 is the SEM figure that adds the variable concentrations inhibitor,
A. add 1 * 10 -7MolL -1Nanometer selenium; B. add 1 * 10 -6MolL -1Nanometer selenium;
C. add 5 * 10 -6MolL -1Nanometer selenium; D. add 1 * 10 -5MolL -1Nanometer selenium;
E. add 2 * 10 -5MolL -1Nanometer selenium; F. add 3 * 10 -5MolL -1Nanometer selenium;
G. add 1 * 10 -4MolL -1Nanometer selenium; H. add 1 * 10 -3MolL -1Nanometer selenium.
Fig. 3 is X-ray diffraction (XRD) figure of calcium oxalate crystals,
Wherein, a. does not have the interpolation inhibitor; B. add 3 * 10 -5MolL -1Nanometer selenium.
Fig. 4 is infrared spectrum (FTIR) figure of calcium oxalate crystals,
Wherein, a. does not have the interpolation inhibitor; B. add 3 * 10 -5MolL -1Nanometer selenium.
Fig. 5 is the volumetric usage ratio that adds vitamin c solution and the selenite solution crystalline SEM figure of CaOxa when being respectively the nanometer selenium that made in 1: 0.5 and 1: 2.
The specific embodiment
Specify embodiments of the present invention below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1:
(15～35 ℃, 1 normal atmosphere) get 4 * 10 at normal temperatures and pressures -4MolL -1Vitamin c solution 25ml add in the volumetric flask of 50ml, drip 2 * 10 -4MolL -1Selenium dioxide solution to graduation mark, shake up gently while dripping, treat that redness no longer changes, promptly obtain 1 * 10 -4MolL -1Nanometer selenium, calcium oxalate crystal inhibitor promptly of the present invention.
In three 25mL volumetric flasks, in each volumetric flask, add 0.375mL 0.02molL -1CaCl 2, 2.5mL 0.02molL -1NaCl, 0.375mL 0.02molL -1Na 2Oxa adds redistilled water to the 20mL, shakes up back solution with 0.22 μ m filtering with microporous membrane, adds an amount of 1 * 10 then successively -4MolL -1Nanometer selenium is diluted to scale with redistilled water, in the last solution that obtains of each volumetric flask, and c (Ca 2+)=c (Oxa 2-)=3 * 10 -4MolL -1, c (NaCl)=0.01molL -1, nanometer selenium concentration is respectively 0,1 * 10 -7With 1 * 10 -6MolL -1(metastable solution is meant the above-mentioned solution that has just prepared to the calcium oxalate metastable solution that above-mentioned configuration obtains, place to be only after 3 days and form stable solution) in the 25mL beaker, carry out crystallization, put into the quartz substrate handled well (with the dense H of 3: 1 (v:v) in beaker bottom in advance 2SO 4: H 2O 2(30%) mixed liquid dipping quartz substrate 1h, supersound washing 10min again after cleaning with redistilled water then).
Crystal formation for preventing that volatilization because of aqueous solvent from causing the system supersaturation to drive, crystal growth is carried out in closed environment, behind the crystal growth 3d, taking-up has the crystalline substrate of CaOxa, in silica gel drier after the drying, with SEM observe its pattern (Fig. 2 a, 2b).
Embodiment 2:
(15～35 ℃, 1 normal atmosphere) get 4 * 10 at normal temperatures and pressures -2MolL -1Vitamin c solution 25ml add in the volumetric flask of 50ml, drip 2 * 10 -2MolL -1Selenium dioxide solution to graduation mark, shake up gently while dripping, treat that redness no longer changes, promptly obtain 1 * 10 -2MolL -1Nanometer selenium, calcium oxalate crystal inhibitor promptly of the present invention.
In two 25mL volumetric flasks, in each volumetric flask, add 0.375mL 0.02molL -1CaCl 2, 2.5mL 0.02molL -1NaCl, 0.375mL 0.02molL -1Na 2Oxa adds redistilled water to the 20mL, shakes up back solution with 0.22 μ m filtering with microporous membrane, adds an amount of 1 * 10 then successively -2MolL -1Nanometer selenium is diluted to scale with redistilled water, in the solution that each volumetric flask obtains at last, and c (Ca 2+)=c (Oxa 2-)=3 * 10 -4MolL -1, c (NaCl)=0.01molL -1, nanometer selenium concentration is respectively 1 * 10 in four volumetric flasks -4With 1 * 10 -3MolL -1, the calcium oxalate metastable solution that above-mentioned preparation obtains carries out crystallization in the 25mL beaker, put into the quartz substrate of handling well (quartz substrate is handled with embodiment 1) in beaker bottom in advance.
Taking-up has the crystalline substrate of CaOxa (environment and standing time are with embodiment 1), in silica gel drier after the drying, with SEM observe its pattern (Fig. 2 g, 2h).
Embodiment 3:
(15～35 ℃, 1 normal atmosphere) get 4 * 10 at normal temperatures and pressures -3MolL -1Vitamin c solution 25ml add in the volumetric flask of 50ml, drip 2 * 10 -3MolL -1Selenium dioxide solution to graduation mark, shake up gently while dripping, treat that redness no longer changes, promptly obtain 1 * 10 -3MolL -1Nanometer selenium, calcium oxalate crystal inhibitor promptly of the present invention.
In four 25mL volumetric flasks, add 0.375mL 0.02molL in each volumetric flask -1CaCl 2, 2.5mL 0.02molL -1NaCl, 0.375mL 0.02molL -1Na 2Oxa adds redistilled water to the 20mL, shakes up back solution with 0.22 μ m filtering with microporous membrane, adds an amount of 1 * 10 then successively -4MolL -1Or 1 * 10 -3MolL -1Nanometer selenium is diluted to scale with redistilled water, in the solution that volumetric flask obtains at last, and c (Ca 2+)=c (Oxa 2-)=3 * 10 -4MolL -1, c (NaCl)=0.01molL -1, nanometer selenium concentration is respectively 5 * 10 in four volumetric flasks -6, 1 * 10 -5, 2 * 10 -5With 3 * 10 -5MolL -1, above-mentioned calcium oxalate metastable solution carries out crystallization in the 25mL beaker, put into the quartz substrate of handling well (quartz substrate is handled with embodiment 1) in beaker bottom in advance.
Environment and standing time are with embodiment 1, with inductive coupling plasma emission spectrograph (ICP-AES) calcium ion concentration is carried out in the supernatant and measure (table 1), taking-up has the crystalline substrate of CaOxa, in silica gel drier after the drying, crystal is carried out XRD test (Fig. 3) and SEM observation (Fig. 2 c～2f), the beaker bottom crystal is carried out FTIR detect (Fig. 4).In order to compare zeroth order selenium and tetravalence selenium inhibitory action, with SeO to calcium oxalate 2Solution is observed relatively (Fig. 1) by SEM in contrast.
Embodiment 4:
(15～35 ℃, 1 normal atmosphere) at normal temperatures and pressures, getting 50ml and 12.5ml concentration respectively is 4 * 10 -3MolL -1Vitamin c solution add in the volumetric flask of 100ml, dripping 25ml concentration respectively is 2 * 10 -3MolL -1Selenium dioxide solution, shake up gently while dripping, be diluted to graduation mark, treat that redness no longer changes with redistilled water, the volumetric usage ratio that promptly obtains vitamin c solution and selenite solution is the nanometer selenium that made in 1: 0.5 and 1: 2, calcium oxalate crystal inhibitor promptly of the present invention.
In two 25mL volumetric flasks, add 0.375mL 0.02molL respectively -1CaCl 2, 2.5mL0.02molL -1NaCl, 0.375mL 0.02molL -1Na 2Oxa adds redistilled water to the 20mL, shakes up back solution with 0.22 μ m filtering with microporous membrane, adds an amount of above-mentioned different volumes then successively than the nanometer selenium that makes, and is diluted to scale with redistilled water, in the solution that each volumetric flask obtains at last, and c (Ca 2+)=c (Oxa 2-)=3 * 10 -4MolL -1, c (NaCl)=0.01molL -1, nanometer selenium concentration all is 1 * 10 in two volumetric flasks -6MolL -1, above-mentioned calcium oxalate metastable solution carries out crystallization in the 25mL beaker, put into the quartz substrate of handling well (quartz substrate is handled with embodiment 1) in beaker bottom in advance.
Taking-up has the crystalline substrate of CaOxa (environment and standing time are with embodiment 1), after the drying, observes its pattern (Fig. 5) with SEM in silica gel drier.
Interpretation:
Table 1 adds the concentration of calcium ion in the variable concentrations nanometer selenium clear liquid
Figure A200810219888D00081
As shown in table 1, along with the increase of nanometer selenium concentration, calcium ion concentration increases in the clear liquid, that is to say that heavy poly-calcium reduces, and proves that nanometer selenium has inhibitory action to calcium oxalate.
As shown in Figure 1, (Fig. 1 a), the CaOxa of formation is not the sharp-pointed three-dimensional COM crystal of corner angle, comprises three dimensional hexagonal, folded type and aggregation mutually, and wherein aggregation occurs big blockly, and size reaches tens microns when having selenium to exist.After the adding nanometer selenium (Fig. 1 b), see obviously that from figure nano level bead is exactly nanometer selenium (a circular mark among the 1b figure).Obvious change all takes place in the crystalline size of CaOxa, pattern and crystalline phase.The part crystal becomes two dimension by three-dimensional, rod-like crystal also occurs, and aggregation extent significantly reduces.Add SeO 2Back (Fig. 1 c), CaOxa crystal accumulation degree also has minimizing to a certain degree, but effect does not have nanometer selenium good.
As shown in Figure 2, phenomenon is consistent with Fig. 1, and also being has the part crystal to become two dimension by three-dimensional, rod-like crystal also occurs, and we can also know and see the existence that the nanometer selenium bead is arranged.Along with nanometer selenium concentration from 1 * 10 -7MolL -1To 3 * 10 -5MolL -1Increase progressively (Fig. 2 a～2f), crystalline aggregation extent descends, the reason that produces this result may be: portion C aOxa crystal to be generated after the nanometer selenium circular owing to add, and adds the existence of nanometer selenium bead, and these sphaerocrystals have hindered the crystalline gathering of CaOxa.Yet, in nanometer selenium concentration 1 * 10 -4, 1 * 10 -3MolL -1The time (Fig. 2 g, 2h), rod-like crystal tails off, and aggregation extent has aggravated again, and the amount of this explanation adding nanometer selenium can not be too much, 3 * 10 -5MolL -1About comparatively suitable.
As shown in Figure 3, for adding and the crystalline XRD figure of CaOxa when not adding nanometer selenium.When not adding nanometer selenium (Fig. 3 a), the main diffraction maximum crystal face of CaOxa is to belong to COM crystalline (101), 202, and and (130) crystal face.Add 3 * 10 -5After the mol/L nanometer selenium (Fig. 3 b), above-mentioned crystal face weakens greatly, COD crystalline (202) and (411) crystal face occurred belonging to.Selenic (210) crystal face has also appearred simultaneously.In conjunction with the result of the crystalline SEM shape appearance figure of CaOxa, we infer that the conglobate crystal of transformation should be the mixed crystal after COD crystal and selenium interact.
As shown in Figure 4, for adding and the crystalline FTIR collection of illustrative plates of CaOxa when not adding nanometer selenium.When not having nanometer selenium to exist (Fig. 4 a), at 662cm -1, 784cm -1, 884cm -1And 944cm -1The place is the characteristic peak of COM.At 3061cm -1To 3488cm -1The water peak of COM, 1323cm appear in the place -1And 1613cm -1The place is the carbonyl of the COM vibration peak that contracts the second month in a season.Can determine that sample is COM, consistent with viewed result (3a) among the XRD.Fig. 4 b is for adding 3 * 10 -5The FTIR spectrum of mol/L nanometer selenium, 3386cm -1The place is the characteristic absorption peak of hydrone among the COD, 1639cm -1Stretching vibration peak for COD carbonyl and C=O.At 1319cm -1Place's its numerical value of peak value all is between COM and the COD characteristic peak, shows that the part crystal that generates this moment is the mixture of COM and COD, and this is consistent with viewed result (3b) among the XRD.At 569cm -1The characteristic peak of C-O-Se has appearred in the place, at 1044cm -1The characteristic peak of Se-O-Se has appearred in the place.Nanometer selenium and Oxa that proof adds 2-Certain interaction is arranged, form the structure of C-O-Se and Se-O-Se.
As shown in Figure 5,5a and 5b are the volumetric usage ratio that adds vitamin c solution and the selenite solution crystalline SEM figure of CaOxa when being respectively the nanometer selenium that made in 1: 0.5 and 1: 2, and dispersion effect is not as Fig. 2.So the volumetric usage of vitamin c solution and selenite solution is better than for 1:1 the time.
To sum up analyze inhibitor of the present invention (nanometer selenium) and can effectively suppress calcium oxalate growth and gathering.Tetravalence selenium also has certain effect, but not as the zeroth order nanometer selenium.
Embodiment 5:
The difference of present embodiment and embodiment 1 to 4 is that a selenium dioxide solution changes sodium selenite solution into, and gained inhibitor performance such as embodiment gained inhibitor are approximate, and concrete data are omitted.

Claims (8)

1, a kind of calcium oxalate crystal inhibitor is characterized in that: be to be made by nanometer selenium.
2, calcium oxalate crystal inhibitor according to claim 1 is characterized in that: described nanometer selenium is by selenite solution and vitamin c solution hybrid reaction and obtain.
3, calcium oxalate crystal inhibitor according to claim 1 is characterized in that: ascorbic concentration is 4 * 10 in the described vitamin c solution -4～4 * 10 -2MolL -1, the concentration of the selenite in the described selenite solution is 2 * 10 -4～2 * 10 -2MolL -1Described vitamin c solution is 1: 0.5～2 with the volumetric usage ratio of selenite solution.
4, calcium oxalate crystal inhibitor according to claim 3 is characterized in that: ascorbic concentration is 4 * 10 in the described vitamin c solution -3MolL -1, the concentration of the selenite solution in the described selenite solution is 2 * 10 -3MolL -1
5, calcium oxalate crystal inhibitor according to claim 3 is characterized in that: described vitamin c solution is 1: 1 with the volumetric usage ratio of selenite solution.
6, calcium oxalate crystal inhibitor according to claim 1 is characterized in that: described selenite is sodium selenite or selenium dioxide.
7, calcium oxalate crystal inhibitor according to claim 1, it is characterized in that: described vitamin C is meant the reduced form vitamin C.
8, the application of each described calcium oxalate crystal inhibitor of claim 1～7 in preparation calcium oxalate stone suppressive drug.
CN2008102198882A 2008-12-12 2008-12-12 Use of nano selenium in preparing calcium oxalate crystallization inhibitor Expired - Fee Related CN101433549B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102293784A (en) * 2011-08-08 2011-12-28 韩洪波 Pearl nano selenium and its preparation method
CN102488706A (en) * 2011-12-23 2012-06-13 上海海洋大学 Medicament for preventing and treating urinary calculus and preparation method and application thereof
CN107640748A (en) * 2017-10-27 2018-01-30 陕西科技大学 A kind of biological synthesis method of nanometer selenium
CN111116354A (en) * 2019-12-17 2020-05-08 天津大学 Application of gallic acid and its derivatives in controlling calcium oxalate crystallization process

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102293784A (en) * 2011-08-08 2011-12-28 韩洪波 Pearl nano selenium and its preparation method
CN102488706A (en) * 2011-12-23 2012-06-13 上海海洋大学 Medicament for preventing and treating urinary calculus and preparation method and application thereof
CN102488706B (en) * 2011-12-23 2013-12-11 上海海洋大学 Medicament for preventing and treating urinary calculus and preparation method and application thereof
CN107640748A (en) * 2017-10-27 2018-01-30 陕西科技大学 A kind of biological synthesis method of nanometer selenium
CN107640748B (en) * 2017-10-27 2020-12-25 陕西科技大学 Biological synthesis method of nano-selenium
CN111116354A (en) * 2019-12-17 2020-05-08 天津大学 Application of gallic acid and its derivatives in controlling calcium oxalate crystallization process
CN111116354B (en) * 2019-12-17 2022-08-09 天津大学 Application of gallic acid and its derivatives in controlling calcium oxalate crystallization process

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