CN100581538C - Magnetic slow releasing diclofenac sodium preparation in supermolecular intercalation structure and its preparation method - Google Patents
Magnetic slow releasing diclofenac sodium preparation in supermolecular intercalation structure and its preparation method Download PDFInfo
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- CN100581538C CN100581538C CN200610165224A CN200610165224A CN100581538C CN 100581538 C CN100581538 C CN 100581538C CN 200610165224 A CN200610165224 A CN 200610165224A CN 200610165224 A CN200610165224 A CN 200610165224A CN 100581538 C CN100581538 C CN 100581538C
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Abstract
The present invention is magnetic slow releasing diclofenac sodium in supermolecular intercalation structure and its preparation process, and belongs to the field of hydrotalcite material technology. The magnetic diclofenac sodium has the chemical expression of (M2+)1-x(N3+)x(OH)2(DIK-)a(Bn-)b.mH2O.kM'Fe2O4, and is prepared through the first coprecipitation process to prepare nanometer magnetic kernel, the subsequent mixing of the magnetic kernel with corresponding salt solution, and the final coprecipitation process to assemble diclofenac sodium into the hydrotalcite layers and to obtain the diclofenac sodium intercalated hydrotalcite with magnetic kernel. The magnetic slow releasing diclofenac sodium in supermolecular intercalation structure has high stability, raised bioavailability, capable of magnetic field location and targeting location and effective control on the medicine structure, composition, etc.
Description
Technical field
The invention belongs to the hydrotalcite material technical field, particularly a kind of magnetic supermolecular intercalation structure slow releasing diclofenac sodium and preparation method thereof.
Background technology
The magnetic slow releasing pharmaceutical be a class set magnetic and sustained release in the medicine of one, after this type of medicine is used in the body, utilize the bootable medicine of external magnetic field effect directed in vivo move and location set in, and realize that controlled delivery of pharmaceutical agents discharges.Therefore, this type of drug main will be used as anti-cancer medicament carrier, and zoopery and clinical observation prove, magnetic and medicated have a definite anticancer growth effect, patient tumors dwindled, subjective symptoms improvement etc.
Existing magnetic slow releasing agent medicine has following two classes: 1) the magnetic slow releasing tablet is to add ferromagnetic powder in slow releasing tablet.Release method is to add slow releasing agent in the tablet or use the slow-release material coating.2) the magnetic slow releasing capsule is a kind of insoluble capsule that has pore, and medicine and ferromagnetic powder material are equipped with in inside; Also Magnaglo can be added in the capsule shells; Also available ferromagnetic material prepares capsule, reinstalls medicine.
Diclofenac sodium (DIK), diclofenac have good pain relieving, bring down a fever and antiphlogistic effects.Antipyretic effect can be reset mainly due to diclofenac and is positioned at hypothalamic temperature control centre, and antiinflammatory and analgesic effect then are because it can effectively stop the generation of prostaglandin.Diclofenac can well pain management and the inflammation for the treatment of rheumatism class and non-rheumatism class on pharmacology.Yet it also has some shortcomings, and such as poorly water-soluble, unstable in aqueous solution, bioavailability is low, and this shortcoming is can't rely on organic polymer commonly used to coat the synthetic sustained release agent of method to solve.Because its half-life has only 1.8 hours,, often need heavy dose and repeatedly take in addition, tend to cause many negative influences if directly oral.Therefore need develop a kind of slow releasing preparation, reduce negative effect.
Based on the defective of traditional diclofenac preparation of sodium, people develop various diclofenac sodium slow releasing preparation.
But still there is not report at present based on magnetic supermolecular intercalation diclofenac sodium slow release formulation.This magnetic intercalation configuration diclofenac sodium not only can be controlled the rate of release of diclofenac sodium, avoids drug release too fast, strengthens its stability, and then improves its bioavailability, and reaches raising dispersibility and the localized effect of targeting by externally-applied magnetic field.
Summary of the invention:
The object of the present invention is to provide a kind of magnetic supermolecular intercalation structure slow releasing diclofenac sodium and preparation method thereof, have magnetic, and have the magnetic intercalation configuration diclofenac sodium slow release formulation that discharges lasting period and rate of release.
The preparation method of magnetic intercalation configuration diclofenac sodium slow release formulation of the present invention: with the diclofenac sodium is the intercalation object, and anion laminated material LDHs is a main body, by the supermolecular intercalation assembling diclofenac sodium is assembled into the LDHs interlayer; Simultaneously, magnetic core is coated on brucite inside, makes it have magnetic.
Magnetic intercalation configuration diclofenac sodium slow releasing agent of the present invention is a supramolecular structure, and its crystal structure is the crystal structure of houghite material, and chemical formula is: (M
2+)
1-x(N
3+)
x(OH)
2(DIK
-)
a(B
N-)
bMH
2OkM ' Fe
2O
4(M wherein
2+)
1-x(N
3+)
x(OH)
2(DIK
-)
a(B
N-)
bMH
2O can be abbreviated as DIK-LDHs, M ' Fe
2O
4Be magnetic species, DIK-LDHs is for being coated on M ' Fe
2O
4Outer diclofenac sodium intercalated houghite.Its quality percentage composition is:
M’Fe
2O
4：1％～10％；
DIK-LDHs:90%～99%; DIK:40%～60% wherein;
M wherein
2+Be bivalent metal ion Mg
2+, Zn
2+In any;
N
3+Be trivalent metal ion Al
3+, Fe
3+In any;
M ' is Mg
2+, Ni
2+, Co
2+Wherein any of bivalent metal ion, M
2+Can be the same or different with M ';
DIK
-Represent interlayer monovalence diclofenac sodium anion;
B
N-For carrying capacity is the inorganic anion of n, B in the DIK-LDHs chemical formula
N-Can not exist or for CO
3 2-, NO
3 -In any, two kinds or three kinds;
X=N
3+/ (M
2++ N
3+), 0＜x＜1; A, b are respectively DIK
-, B
N-Quantity, and satisfy a+n * b=x, m is the crystallization water number, 0＜m＜5; K is M ' Fe
2O
4Numerator coefficients.
Magnetic diclofenac sodium slow releasing agent is a kind of medicine-hydrotalcite composite material with magnetic, and the quality percentage composition of diclofenac sodium is 40～60% in this slow releasing agent; The quality percentage composition of water is 2～15%; The slow release lasting period is 1～15h; Specific saturation magnetization is 2～10AM
2/ Kg.
The concrete preparation process of magnetic intercalation configuration diclofenac sodium slow release formulation of the present invention is:
A, nano-magnetic nuclear M ' Fe
2O
4Powder preparing
(1) .MgFe
2O
4: take by weighing Mg (NO
3)
26H
2O, Fe (NO
3)
39H
2O and FeCl
24H
2O is made into mixing salt solution, wherein (Mg
2++ Fe
2+)/Fe
3+Mol ratio is 3, Mg
2+/ Fe
2+Mol ratio is 1; Mg
2+Molar concentration be 0.1～2.5Mol/L, Fe
3+Molar concentration be 0.2～5.0Mol/L; Take by weighing NaOH and Na
2CO
3Be made into mixed ammonium/alkali solutions; Wherein the NaOH molar concentration is 0.1～5.0Mol/L; Na
2CO
3Molar concentration is 0.5～0.8Mol/L.
(2) .NiFe
2O
4: the soluble inorganic salt and two of M ', ferric soluble inorganic salt are mixed with mixed solution, wherein (Ni
2++ Fe
2+)/Fe
3+Mol ratio is 3, Ni
2+/ Fe
2+Mol ratio is 1; Ni
2+Molar concentration be 0.1～2.5Mol/L, Fe
3+Molar concentration be 0.2～5.0Mol/L; Preparation NaOH aqueous slkali, wherein the NaOH molar concentration is 0.1～5.0Mol/L;
Under nitrogen protection alkali liquor splashed in the saline solution to pH value and equal 7～11,30～60 ℃ of crystallization are 4～10 hours in water-bath, with the reactant liquor sucking filtration, with taking off CO
2Deionized water wash, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, obtains particle size range in 6～9 hours at the M ' of 100～600nm Fe through 800～1200 ℃ of high-temperature roastings
2O
4Powder body.Obtain powder body uniformly with the standard screen screening.All reactant liquors and slurry are all used the carbon dioxide removal deionized water.
The preparation of b, magnetic diclofenac sodium intercalated houghite
Step 1: divalent metal salt and trivalent metal salt are pressed M
2+/ N
3+=2～4 mol ratio is made into mixing salt solution A with the carbon dioxide removal deionized water, presses divalent metal nitrate and M ' Fe
2O
4Mass ratio be 54: 1～13.5: 1 with M ' Fe
2O
4Join in the solution A, the concentration of solution A is 0.1～1Mol/L; In addition diclofenac sodium is dissolved in the NaOH solution, the preparation solution B, wherein the concentration of NaOH is 1Mol/L, the concentration of diclofenac sodium is 0.1Mol/L;
M wherein
2+Can be Mg
2+, Zn
2+In any, N
3+Can be Al
3+, Fe
3+In any, soluble M
2+, N
3+The anion of salt can be NO
3 -, Cl
-
Step 2: with the reaction vessel that solution A places band to stir, be under 0.01～0.5ml/s condition mixed ammonium/alkali solutions B slowly to be added, stop between 7.8～12.8 to the pH of gained serosity, change in the crystallizing kettle in drop rate;
Step 3: in crystallizing kettle, use N
2Protection makes serosity crystallization 8～24 hours under 40～80 ℃ of temperature, again through sucking filtration, be washed to neutrality, vacuum drying 20～48 hours obtains DIK-LDHs/M ' Fe
2O
4
The quality percentage composition of diclofenac sodium is 40～60% in this slow releasing agent; The quality percentage composition of water is 2～15%; The slow release lasting period is 1～15 hour; Specific saturation magnetization is 2～10AM
2/ Kg.
Reactant liquor and slurries all in step 1～3 are all used the carbon dioxide removal deionized water.
Advantage of the present invention is:
[1] prepares a kind of new magnetic supermolecular intercalation structure slow releasing diclofenac sodium, can control the diclofenac sodium rate of release.Because the diclofenac sodium intercalation in hydrotalcite layers, can strengthen its stability, improves its bioavailability, and reach raising dispersibility and the localized effect of targeting by externally-applied magnetic field.
[2] first the supermolecular intercalation assemble method is used to prepare the magnetic slow releasing diclofenac sodium.
[3] by adjusting the assembling condition of DIK-LDHs, as changing M
2+/ M
3+Type and mol ratio, adjusting magnetic core M ' Fe
2O
4Kind and pH value of mole, crystallization process and terminal point, crystallization temperature, crystallization time etc., can realize control to DIK-LDHs structure, composition, burst size, release lasting period and magnetic size.
The specific embodiment:
Embodiment 1
(1) magnetic core MgFe
2O
4The preparation of nano-powder
Take by weighing 5.128g (0.02Mol) Mg (NO
3)
26H
2O, 4.04g (0.01Mol) Fe (NO
3)
39H
2O and 1.99g (0.01Mol) FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6g (0.15Mol) NaOH and 7.42g (0.07Mol) Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Aqueous slkali dropwise splashed in the mixing salt solution to pH value equal 11,40 ℃ of crystallization are 10 hours in water-bath, with the reactant liquor sucking filtration, washing, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, roasting 8 hours in 800 ℃, air atmosphere again, 10 ℃/minute of heating rates make magnetic nuclear MgFe
2O
4Obtain powder body uniformly with the standard screen screening.Institute's water is the carbon dioxide removal deionized water in the process.
(2) preparation of magnetic diclofenac sodium intercalation magnesium aluminum-hydrotalcite
Take by weighing Mg (NO
3)
26H
2O (0.02Mol), Al (NO
3)
39H
2O (0.01Mol) is dissolved in wiring solution-forming A in the 80ml carbon dioxide removal deionized water.At N
2Under the gas shiled, pour in the four-hole boiling flask, other adds magnetic nuclear MgFe
2O
40.0949g, Mg (NO
3)
26H
2O/MgFe
2O
4Mass ratio is 54.00.Weighing 4.00g (0.1Mol) NaOH in addition, 3.18g (0.01Mol) diclofenac sodium is configured to the mixed ammonium/alkali solutions of 150ml, dropwise is added dropwise in the four-hole boiling flask, titration end-point pH value to 12.8, the gained serosity is in N
2Protection down, 70 ℃ of crystallization 72 hours.Through sucking filtration, washing is to neutrality, room temperature vacuum drying 48 hours again.Institute's water is the carbon dioxide removal deionized water in the process.
The magnetic coercive force Hc value that records this sample is 0kA/m, specific saturation magnetization б
xBe 4.13AM
2/ Kg; Chemical composition is [Mg
0.69Al
0.31(OH)
2] (DIK)
0.31H
2O0.0273MgFe
1.10O
2.15, the content of diclofenac is about 54.22% in this product.
Embodiment 2
(1) magnetic core MgFe
2O
4The preparation of nano-powder
Take by weighing 5.128g (0.02Mol) Mg (NO
3)
26H
2O, 4.04g (0.01Mol) Fe (NO
3)
39H
2O and 1.99g (0.01Mol) FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6g (0.15Mol) NaOH and 7.42g (0.07Mol) Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Aqueous slkali dropwise splashed in the mixing salt solution to pH value equal 11,40 ℃ of crystallization are 10 hours in water-bath, with the reactant liquor sucking filtration, washing, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, roasting 8 hours in 800 ℃, air atmosphere again, 10 ℃/minute of heating rates make magnetic nuclear MgFe
2O
4Obtain powder body uniformly with the standard screen screening.Institute's water is the carbon dioxide removal deionized water in the process.
(2) preparation of magnetic intercalation diclofenac sodium magnesium aluminum-hydrotalcite
Take by weighing Mg (NO
3)
26H
2O (0.02Mol), Al (NO
3)
39H
2O (0.01Mol) is dissolved in wiring solution-forming A in the 80ml carbon dioxide removal deionized water.At N
2Under the gas shiled, pour in the four-hole boiling flask, other adds magnetic nuclear MgFe
2O
40.1899g, Mg (NO
3)
26H
2O/MgFe
2O
4Mass ratio is 27.00.Weighing 4.00g (0.1Mol) NaOH in addition, 3.18g (0.01Mol) diclofenac sodium is configured to the mixed ammonium/alkali solutions of 150ml, dropwise is added dropwise in the four-hole boiling flask, titration end-point pH value to 12.8, the gained serosity is in N
2Protection down, 70 ℃ of crystallization 72 hours.Through sucking filtration, washing is to neutrality, room temperature vacuum drying 48 hours again.Institute's water is the carbon dioxide removal deionized water in the process.
The magnetic coercive force Hc value that records this sample is 0kA/m, specific saturation magnetization б
xBe 4.87AM
2/ Kg; Chemical composition is [Mg
0.70Al
0.30(OH)
2] (DIK)
0.350.75H
2O0.051MgFe
1.10O
2.15, diclofenac content is about 56.80% in this product.
Embodiment 3
(1) magnetic core MgFe
2O
4The preparation of nano-powder
Take by weighing 5.128g (0.02Mol) Mg (NO
3)
26H
2O, 4.04g (0.01Mol) Fe (NO
3)
39H
2O and 1.99g (0.01Mol) FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6g (0.15Mol) NaOH and 7.42g (0.07Mol) Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Aqueous slkali dropwise splashed in the mixing salt solution to pH value equal 11,40 ℃ of crystallization are 10 hours in water-bath, with the reactant liquor sucking filtration, washing, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, roasting 8 hours in 800 ℃, air atmosphere again, 10 ℃/minute of heating rates make magnetic nuclear MgFe
2O
4Obtain powder body uniformly with the standard screen screening.Institute's water is the carbon dioxide removal deionized water in the process.
(2) preparation of magnetic intercalation diclofenac sodium magnesium aluminum-hydrotalcite
Take by weighing Mg (NO
3)
26H
2O (0.02Mol), Al (NO
3)
39H
2O (0.01Mol) is dissolved in wiring solution-forming A in the 80ml carbon dioxide removal deionized water.At N
2Under the gas shiled, pour in the four-hole boiling flask, other adds magnetic nuclear MgFe
2O
40.3799g, Mg (NO
3)
26H
2O/MgFe
2O
4Mass ratio is 13.5.Weighing 4.00g (0.1Mol) NaOH in addition, 3.18g (0.01Mol) diclofenac sodium is configured to the mixed ammonium/alkali solutions of 150ml, dropwise is added dropwise in the four-hole boiling flask, titration end-point pH value to 12.8, the gained serosity is in N
2Protection down, 70 ℃ of crystallization 72 hours.Through sucking filtration, washing is to neutrality, room temperature vacuum drying 48 hours again.Institute's water is the carbon dioxide removal deionized water in the process.
The magnetic coercive force Hc value that records this sample is 0kA/m, specific saturation magnetization б
xBe 6.11AM
2/ Kg; Chemical composition is [Mg
0.70Al
0.30(OH)
2] (DIK)
0.32H
2O0.108MgFe
1.10O
2.15, the content of diclofenac is about 51.23% in this product.
Embodiment 4
(1) magnetic core MgFe
2O
4The preparation of nano-powder
Take by weighing 5.128g (0.02Mol) Mg (NO
3)
26H
2O, 4.04g (0.01Mol) Fe (NO
3)
39H
2O and 1.99g (0.01Mol) FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6g (0.15Mol) NaOH and 7.42g (0.07Mol) Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Aqueous slkali dropwise splashed in the mixing salt solution to pH value equal 11,40 ℃ of crystallization are 10 hours in water-bath, with the reactant liquor sucking filtration, washing, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, roasting 8 hours in 800 ℃, air atmosphere again, 10 ℃/minute of heating rates make magnetic nuclear MgFe
2O
4Obtain powder body uniformly with the standard screen screening.Institute's water is the carbon dioxide removal deionized water in the process
(2) preparation of magnetic diclofenac sodium intercalation zinc-aluminium brucite
Take by weighing Zn (NO
3)
26H
2O (0.02mol), Al (NO
3)
39H
2O (0.01mol) is dissolved in wiring solution-forming A in the 80ml water.At N
2Under the gas shiled, pour in the four-hole boiling flask, other adds magnetic nuclear MgFe
2O
40.1102g, Zn (NO
3)
26H
2O/MgFe
2O
4Mass ratio is 54.Weighing 4.00g (0.1Mol) NaOH in addition, 3.18g (0.01Mol) diclofenac sodium is configured to the mixed ammonium/alkali solutions of 150ml, dropwise is added dropwise in the four-hole boiling flask, titration end-point pH value to 7.8, the gained serosity is in N
2Protection down, 70 ℃ of crystallization 72 hours.Through sucking filtration, washing is to neutrality, room temperature vacuum drying 48 hours again.Institute's water is the carbon dioxide removal deionized water in the process.
The magnetic coercive force Hc value that records this sample is 0kA/m, specific saturation magnetization б
xBe 4.22AM
2/ Kg; Chemical composition is [Zn
0.65Al
0.35(OH)
2] (DIK)
0.351.21H
2O0.021MgFe
2O
4, the content of diclofenac sodium is 48.42%.
Embodiment 5
(1) magnetic core MgFe
2O
4The preparation of nano-powder
Take by weighing 5.128g (0.03Mol) Mg (NO
3)
26H
2O, 4.04g (0.01Mol) Fe (NO
3)
39H
2O and 1.99g (0.01Mol) FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6g (0.15Mol) NaOH and 7.42g (0.07Mol) Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Aqueous slkali dropwise splashed in the mixing salt solution to pH value equal 11,40 ℃ of crystallization are 10 hours in water-bath, with the reactant liquor sucking filtration, washing, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, roasting 8 hours in 800 ℃, air atmosphere again, 10 ℃/minute of heating rates make magnetic nuclear MgFe
2O
4Obtain powder body uniformly with the standard screen screening.Institute's water is the carbon dioxide removal deionized water in the process.
(2) preparation of magnetic diclofenac sodium intercalation zinc-aluminium brucite
Take by weighing Zn (NO
3)
26H
2O (0.04mol), Al (NO
3)
39H
2O (0.01mol) is dissolved in wiring solution-forming A in the 80ml water.At N
2Under the gas shiled, pour in the four-hole boiling flask, other adds magnetic nuclear MgFe
2O
40.1653g, Zn (NO
3)
26H
2O/MgFe
2O
4Mass ratio is 27.Weighing 4.00g (0.1Mol) NaOH in addition, 3.18g (0.01Mol) diclofenac sodium is configured to the mixed ammonium/alkali solutions of 150ml, dropwise is added dropwise in the four-hole boiling flask, titration end-point pH value to 7.8, the gained serosity is in N
2Protection down, 70 ℃ of crystallization 72 hours.Through sucking filtration, washing is to neutrality, room temperature vacuum drying 48 hours again.Institute's water is the carbon dioxide removal deionized water in the process.
The magnetic coercive force Hc value that records this sample is 0kA/m, specific saturation magnetization б
xBe 5.04AM
2/ Kg; Chemical composition is [Zn
0.68Al
0.32(OH)
2] (DIK)
0.370.89H
2O0.048MgFe
2O
4, the content of diclofenac sodium is 50.12%.
Embodiment 6
(1) magnetic core MgFe
2O
4The preparation of nano-powder
Take by weighing 5.128g (0.02Mol) Mg (NO
3)
26H
2O, 4.04g (0.01Mol) Fe (NO
3)
39H
2O and 1.99g (0.01Mol) FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6g (0.15Mol) NaOH and 7.42g (0.07Mol) Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Aqueous slkali dropwise splashed in the mixing salt solution to pH value equal 11,40 ℃ of crystallization are 10 hours in water-bath, with the reactant liquor sucking filtration, washing, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, roasting 8 hours in 800 ℃, air atmosphere again, 10 ℃/minute of heating rates make magnetic nuclear MgFe
2O
4Obtain powder body uniformly with the standard screen screening.Institute's water is the carbon dioxide removal deionized water in the process.
(2) preparation of magnetic diclofenac sodium intercalation zinc-aluminium brucite
Take by weighing Zn (NO
3)
26H
2O (0.04mol), Al (NO
3)
39H
2O (0.01mol) is dissolved in wiring solution-forming A in the 80ml water.At N
2Under the gas shiled, pour in the four-hole boiling flask, other adds magnetic nuclear MgFe
2O
40.2203g, Zn (NO
3)
26H
2O/MgFe
2O
4Mass ratio is 13.5.Weighing 4.00g (0.1Mol) NaOH in addition, 3.18g (0.01Mol) diclofenac sodium is configured to the mixed ammonium/alkali solutions of 150ml, dropwise is added dropwise in the four-hole boiling flask, titration end-point pH value to 7.8, the gained serosity is in N
2Protection down, 70 ℃ of crystallization 72 hours.Through sucking filtration, washing is to neutrality, room temperature vacuum drying 48 hours again.Institute's water is the carbon dioxide removal deionized water in the process.The magnetic coercive force Hc value that records this sample is 0kA/m, specific saturation magnetization б
xBe 6.21AM
2/ Kg; Chemical composition is [Zn
0.71Al
0.29(OH)
2] (DIK)
0.288(CO
3)
0.011.07H
2O0.097MgFe
2O
4, the content of diclofenac sodium is 41.55%.
Claims (2)
1. magnetic supermolecular intercalation structure slow releasing diclofenac sodium, its crystal structure is the crystal structure of houghite material, it is characterized in that: chemical formula is: (M
2+)
1-x(N
3+)
x(OH)
2(DIK
-)
a(B
N-)
bMH
2OkM ' Fe
2O
4(M wherein
2+)
1-x(N
3+)
x(OH)
2(DIK
-)
a(Bn
-)
bMH
2O is abbreviated as DIK-LDHs, M ' Fe
2O
4Be magnetic species, DIK-LDHs is for being coated on M ' Fe
2O
4Outer diclofenac sodium intercalated houghite; Its quality percentage composition is: M ' Fe
2O
4: 1%～10%; DIK-LDHs:90%～99%, wherein, DIK:40%～60%; M
2+Be bivalent metal ion Zn
2+, Mg
2+In any; N
3+Be trivalent metal ion Al
3+, Fe
3+In any; M ' is Mg
2+, Ni
2+Wherein any of bivalent metal ion, M
2+Identical or different with M '; DIK
-Represent interlayer monovalence ibuprofen anion; B
N-For carrying capacity is the inorganic anion of n, B in the DIK-LDHs chemical formula
N-Can not exist or for CO
3 2-, NO
3 -In 1～2 kind; X=N
3+/ (M
2++ N
3+), 0＜x＜1; A, b are respectively DIK
-, B
N-Quantity, and satisfy a+n * b=x, m is the crystallization water number, 0＜m＜5, k is M ' Fe
2O
4Numerator coefficients.
2. preparation method for preparing the described magnetic supermolecular intercalation structure of claim 1 slow releasing diclofenac sodium, adopt coprecipitation to prepare nano-scale magnetic nuclear earlier, with this magnetic core and corresponding salt solution mix, diclofenac sodium is assembled into hydrotalcite layers, obtains having the diclofenac sodium intercalated houghite of magnetic simultaneously; Technology is:
(1) nano-magnetic nuclear M ' Fe
2O
4Powder preparing
A, MgFe
2O
4: take by weighing Mg (NO
3)
26H
2O, Fe (NO
3)
39H
2O and FeCl
24H
2O is made into mixing salt solution, wherein (Mg
2++ Fe
2+)/Fe
3+Mol ratio is 3, Mg
2+/ Fe
2+Mol ratio is 1; Mg
2+Molar concentration be 0.1～2.5Mol/L, Fe
3+Molar concentration be 0.2～5.0Mol/L; Take by weighing NaOH and Na
2CO
3Be made into mixed ammonium/alkali solutions; Wherein, the NaOH molar concentration is 0.1～5.0Mol/L; Na
2CO
3Molar concentration is 0.5～0.8Mol/L;
B, NiFe
2O
4: the soluble inorganic salt and two of M ', ferric soluble inorganic salt are mixed with mixed solution, wherein (Ni
2++ Fe
2+)/Fe
3+Mol ratio is 3, Ni
2+/ Fe
2+Mol ratio is 1; Ni
2+Molar concentration be 0.1～2.5Mol/L, Fe
3+Molar concentration be 0.2～5.0Mol/L; Preparation NaOH aqueous slkali, wherein the NaOH molar concentration is 0.1～5.0Mol/L;
C, under nitrogen protection alkali liquor splashed in the saline solution to pH value 7～11,30～60 ℃ of crystallization are 4～10 hours in water-bath, with the reactant liquor sucking filtration, with taking off CO
2Deionized water wash, the reuse absolute ethanol washing, grinds to form powdery at vacuum drying, obtains particle size range in 6～9 hours at the M ' of 100～600nm Fe through 800～1200 ℃ of high-temperature roastings
2O
4Powder body; Obtain powder body uniformly with the standard screen screening, all reactant liquors and slurry are all used the carbon dioxide removal deionized water;
(2) preparation of magnetic diclofenac sodium intercalated houghite
Step 1: divalent metal salt and trivalent metal salt are pressed M
2+/ N
3+=2～3 mol ratio is made into mixing salt solution A with the carbon dioxide removal deionized water, presses divalent metal nitrate and M ' Fe
2O
4Mass ratio be 54: 1～13.5: 1 with M ' Fe
2O
4Join in the solution A, the concentration of solution A is 0.1～1Mol/L; In addition diclofenac sodium is dissolved in the NaOH solution, the preparation solution B, wherein the concentration of NaOH is 1Mol/L, the concentration of diclofenac sodium is 0.1Mol/L;
M wherein
2+Be Mg
2+, Zn
2+In any, N
3+Be Al
3+, Fe
3+In any, soluble M
2+, N
3+The anion of salt is NO
3 -, Cl
-
Step 2: with the reaction vessel that solution A places band to stir, be under 0.01～0.5ml/s condition mixed ammonium/alkali solutions B to be added, stop between 7.8～12.8 to the pH of gained serosity, change in the crystallizing kettle in drop rate;
Step 3: in crystallizing kettle, use N
2Protection makes serosity crystallization 8～24 hours under 40～80 ℃ of temperature, again through sucking filtration, be washed to neutrality, vacuum drying 20～48 hours obtains DIK-LDHsM ' Fe
2O
4Reactant liquor and slurries all in step 1～3 are all used the carbon dioxide removal deionized water.
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Non-Patent Citations (2)
| Title |
|---|
| 磁性药物－无机纳米复合材料的结构设计与表征. 孙辉等.科学通报，第49卷第24期. 2004 |
| 磁性药物－无机纳米复合材料的结构设计与表征. 孙辉等.科学通报，第49卷第24期. 2004 * |
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|---|---|---|---|---|
| CN101850123A (en) * | 2010-06-10 | 2010-10-06 | 北京化工大学 | Inorganic nano hybrid material of nuclear-shell-type fluorescent-labeled magnetic medicine and preparation method thereof |
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