CN104402705B - Spherical calcium citrate, and preparation method and application thereof - Google Patents
Spherical calcium citrate, and preparation method and application thereof Download PDFInfo
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- CN104402705B CN104402705B CN201410612039.9A CN201410612039A CN104402705B CN 104402705 B CN104402705 B CN 104402705B CN 201410612039 A CN201410612039 A CN 201410612039A CN 104402705 B CN104402705 B CN 104402705B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/12—Carboxylic acids; Salts or anhydrides thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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Abstract
The invention belongs to the field of calcium citrate, and concretely relates to spherical calcium citrate, and a preparation method and application thereof. The provided calcium citrate is spherical, has the diameter of 10-100 mu m and has the specific surface area of 1-80 m＜2＞/g determined by a BET method. The prepared spherical calcium citrate is calcium citrate with a new morphology never reported before, calcium citrate, which is extremely good in biocompatibility, is endowed with new performances, and the application scope of calcium citrate is expanded. The foreseeable thing is that if the morphology of calcium citrate can be effectively controlled and calcium citrate powders with diversified morphologies can be obtained, calcium citrate powders with different properties can be obtained and the application fields of calcium citrate can be expanded.
Description
Technical field
The invention belongs to calcium citrate field, and in particular to a kind of spherical calcium citrate and its preparation method and application.
Background technology
Calcium citrate is a kind of extraordinary organic calcium salt of biocompatibility, is easily absorbed by the body due to which, nontoxic
Advantage, calcium citrate are often used as the calcium deficiency diseases such as calsium supplement, treatment osteoporosis.Calcium citrate typically passes through hydroxide
Calcium and citric acid acid-base titration or Calcium Carbonate and citric acid reactions are obtained, and pay attention to the cheap cheap of raw material, so as to business metaplasia
Produce, but the pattern and crystallization of calcium citrate are not controlled.Such as Chinese patent application 200710021894.2《It is a kind of to utilize
Potato slag method for extracting soluble calcium citrate》, be potato slag to be fermented using Aspergillus niger, obtain citric acid, then with carbon
Sour calcium is reacted；Chinese patent application 201010237025.5《A kind of side that calcium citrate is prepared by Concha Ostreae and scallop shell
Method》, it is preparing calcium citrate using Calcium Carbonate contained in relatively inexpensive Concha Ostreae and scallop shell for raw material.These methods
The characteristics of be raw material sources extensively, low price, be suitable to large-scale industrial production, focus on cost.
In recent years due to noticing nontoxic degradable characteristic in the good biocompatibility of calcium citrate and human body,
Have tried to calcium citrate as bone renovating material.As fourth show it is bright et al.《Simulated body fluid infusion method evaluates calcium citrate
Biological characteristicses》It is middle to be ground, sieved with citric acid reactions, then process using natural Concha Ostreae after crushed, obtain calcium citrate
Granule.Wear star to exist《The development of biotype calcium citrate bone material and correlational study》In also with Concha Ostreae as calcium source and lemon
Lemon acid reaction to calcium citrate, obtain being adapted to the calcium citrate granule of size through screening.
The calcium citrate for using at present is shaped as lamellar, powder, without the relevant report of spherical calcium citrate.
The content of the invention
The technical problem to be solved is to provide a kind of spherical calcium citrate, and the calcium citrate can be used as common lemon
Lemon acid calcium is used, further, since which constitutes spherical structure by lamellar calcium citrate, with high-specific surface area, be calcium citrate this
The fabulous material of one biocompatibility gives new performance, by the range of application of extension calcium citrate.
The present invention provides a kind of spherical calcium citrate, and its a diameter of 10-100 μm (micron), the calcium citrate are based on BET
The specific surface area that method is determined is 1～80m2/g。
Preferably, the calcium citrate is 1～51m based on the specific surface area that BET method is determined2/g。
Preferably, a diameter of 30-60 μm of the spherical calcium citrate.
Further, above-mentioned spherical calcium citrate is formed by lamellar calcium citrate self assembly.
Present invention also offers the preparation method of above-mentioned spherical calcium citrate, by water-soluble Ca salt and water-soluble citrate
Add water be uniformly mixed so as to obtain the mixed aqueous solution of the mixed aqueous solution of calcium salt and citrate, calcium salt and citrate in 40-99 DEG C plus
Thermal agitation 2min-30min, by resulting solidliquid mixture solid-liquid separation, washs and is dried to obtain spherical calcium citrate；Its
In, in the mixed aqueous solution of calcium salt and citrate, in molar ratio, 2.5 ︰ 2 of Gai Li ︰ citrates ＞.
Preferably, in the mixed aqueous solution of calcium salt and citrate, in molar ratio, Gai Li ︰ citrate=2.8～
3.2 ︰ 2.
The water-soluble Ca salt is calcium chloride, at least one in calcium nitrate.
The water-soluble citrate is trisodium citrate, potassium citrate, at least one in Triammonium citrate.
Preferably, in the preparation method of the spherical calcium citrate, heated and stirred speed is 5-60 rev/min.
Further, in above-mentioned spherical calcium citrate preparation method, after heated and stirred before gained solidliquid mixture solid-liquid separation
It is cooled to room temperature.
Preferably, in the preparation method of the spherical calcium citrate, using cryodesiccated method.
Further, the invention provides the application of above-mentioned spherical calcium citrate：Obtained by of the invention, spherical calcium citrate has
All purposes (such as calsium supplement, food additive etc.) of existing calcium citrate, further, since which is spherical and has high-ratio surface
Product, which may be additionally used for：Drug release, Bone Defect Repari etc..
Beneficial effects of the present invention：
The spherical calcium citrate that the present invention is prepared, this is the new pattern of the calcium citrate of no one's report in the past, is Fructus Citri Limoniae
The fabulous material of this biocompatibility of sour calcium gives new performance, by the range of application of extension calcium citrate.It is contemplated that, such as
Fruit then can be obtained dissimilarity with the pattern of effective control calcium citrate so as to obtain the diversified calcium citrate powder body of pattern
The calcium citrate powder body of matter simultaneously will be enlarged by the application of calcium citrate.
Description of the drawings：
The SEM photograph of spherical calcium citrates of the Fig. 1 to prepare in the embodiment of the present invention 1.
Fig. 2 is the SEM photograph of the spherical calcium citrate for preparing under × 1500 amplifications in the embodiment of the present invention 3.
Fig. 3 is the SEM photograph of the spherical calcium citrate for preparing under × 3000 amplifications in the embodiment of the present invention 3.
Fig. 4 is the drug release patterns figure of spherical calcium citrate obtained by test example of the present invention 1.
The XRD figure of spherical calcium citrates of the Fig. 5 to prepare in the embodiment of the present invention 1.
Specific embodiment：
The present invention provides a kind of spherical calcium citrate, and its a diameter of 10-100 μm (micron), the calcium citrate are based on BET
The specific surface area that method is determined is 1～80m2/g。
Preferably, a diameter of 30-60 μm of the spherical calcium citrate.
Above-mentioned spherical calcium citrate is formed by lamellar calcium citrate self assembly.Detailed process is：Calcium salt-citric acid is heated first
Mixed salt solution, separates out lamellar calcium citrate, and the size of the lamellar calcium citrate is about 10-30nm × 20-1000nm × 30-
2000nm, these tablets are mutually attracting with the group such as OH- in electrostatic or calcium citrate, O-Ca-O, hydrogen bond etc. due to itself
Draw near aggregate is formed, also due to tablet belongs to nano material, due to its higher surface activity, nano material is easily rolled into a ball
Ball is polymerized to reduce surface energy, so the lamellar calcium citrate separated out after heating can spontaneous reunion balling-up in the solution.
Present invention also offers the preparation method of above-mentioned spherical calcium citrate, by water-soluble Ca salt and water-soluble citrate
Add water be uniformly mixed so as to obtain the mixed aqueous solution of the mixed aqueous solution of calcium salt and citrate, calcium salt and citrate in 40-99 DEG C plus
Thermal agitation 2min-30min, by resulting solidliquid mixture solid-liquid separation, washs and is dried to obtain spherical calcium citrate；Its
In, in the mixed aqueous solution of calcium salt and citrate, in molar ratio, 2.5 ︰ 2 of Gai Li ︰ citrates ＞；Preferably, calcium from
Sub- ︰ citrate=2.8～8 ︰ 2；It is furthermore preferred that Gai Li ︰ citrate=2.8～3.2 ︰ 2.
In the present invention, calcium citrate can be separated out in calcium salt-citrate solution more than 40 degree, because calcium salt, Fructus Citri Limoniae
Hydrochlorate uses water dissolution, therefore the general boiling point no more than water of temperature；It is easier to form scattered if temperature is too low
Shape calcium citrate, the effect of reunion balling-up are bad.In addition, heat time heating time is shorter, the self-assembly microspheres of formation are less, and the time is longer
Microsphere is bigger.And it was found that, heat time heating time is long, lamellar calcium citrate gradually can be changed into strip by lamellar, because
This time is not more than 30min.
Preferably, in above-mentioned preparation method, Gai Li ︰ citrate=2.8～8 ︰ 2.
Preferably, in the mixed aqueous solution of calcium salt and citrate, in molar ratio, Gai Li ︰ citrate=2.8～
3.2 ︰ 2.
Preferably, in the preparation method of the spherical calcium citrate, heated and stirred speed is 5-60 rev/min.
Stirring mainly makes lamellar calcium citrate obtain the external force of the outside upset for providing, and makes assembling more neat, Bu Huixian
Obtain disorderly and unsystematic；Mixing speed may make very much lamellar calcium citrate easily be adsorbed in chamber wall or bottom slowly, reduce balling-up efficiency；Too
It is fast then self-assembly microspheres may be broken up, 5-60 rev/min.
Preferably, in the preparation method of the spherical calcium citrate, using cryodesiccated method.
The present invention can separate out the calcium citrate of lamellar when being and heating at a temperature of 40-99 DEG C using citrate and calcium salt
Microgranule, under the molecular link and electrostatic interaction in these microgranules, lamellar calcium citrate can be agglomerated into the microsphere of certain pattern automatically.
As the time is longer, the calcium citrate microsphere of reunion can be bigger, therefore, it can control water bath time to reach control calcium citrate
The purpose of self-assembly microspheres size.About 5 microns of microsphere diameter when heating 2 minutes, about 10 microns of microsphere diameter when 5 minutes, 30 points
During clock, microsphere diameter can reach about 30 microns.Because take out after the short periods such as water-bath 2min to have surplus heat, now calcium citrate
Still may proceed to separate out, preferably after the completion of heating add cold water to be cooled down immediately.Further, since vacuum drying easily makes citric acid
Calcium powder is reunited and is lumpd, therefore drying meanss preferably select lyophilization.
Further, the invention provides the application of above-mentioned spherical calcium citrate：Obtained by of the invention, spherical calcium citrate has
All purposes (such as calsium supplement, food additive etc.) of existing calcium citrate, further, since which is spherical, which may be additionally used for：
Drug release, Bone Defect Repari etc..
Embodiment 1
0.8670 gram of CaCl is weighed respectively2, 1.4854 grams of Na3C6H5O7·2H2O, respectively plus 20ml water dissolutioies are in beaker；Will
Na3C6H5O7·2H2O solution adds CaCl2, stir；The beaker that will be equipped with mixed solution is put in water-bath, bath temperature
For 75 degrees Celsius, mixing speed is set to 20r/min；Beaker is taken out after 2 minutes, in beaker, adds distillation to be water-cooled to room temperature
(it is due to slower from 75 degree of natural cooling times, oversize with respect to for the 2min of water-bath, to make the end just addition cold water that is swift in response
It is rapid to lower the temperature)；Filter, solid-liquid separation, take lyophilization after solid washs 3 times, you can obtain the spherical calcium citrate of self assembly, its
SEM figures are as shown in Figure 1；Its a diameter of 10-20 micron.Its specific surface area is 1.737m using the test of BET methods2/g.Gained lemon
The XRD figure of lemon acid calcium is as shown in Figure 5.
Embodiment 2
0.8670 gram of CaCl is weighed respectively2, 1.4854 grams of Na3C6H5O7·2H2O, respectively plus 20ml water dissolutioies are in beaker；Will
Na3C6H5O7·2H2O solution adds CaCl2Solution, stirs；The beaker that will be equipped with mixed solution is put in water-bath, water-bath
Temperature is 75 degrees Celsius, and mixing speed is set to 20r/min；Beaker is taken out after 5 minutes, in beaker, adds distillation to be water-cooled to room
Temperature；Filter, solid-liquid separation, take lyophilization after solid washs 3 times, you can obtain the spherical calcium citrate of self assembly, schemed by its SEM
Understand its a diameter of 10-20 micron.Its specific surface area is 50.824m using the test of BET methods2/g。
Embodiment 3
0.8670 gram of CaCl is weighed respectively2, 1.4854 grams of Na3C6H5O7·2H2O, respectively plus 20ml water dissolutioies are in beaker；Will
Na3C6H5O7·2H2O solution adds CaCl2Solution, stirs；The beaker that will be equipped with mixed solution is put in water-bath, water-bath
Temperature is 75 degrees Celsius, and mixing speed is set to 5r/min；Beaker is taken out after 20 minutes, in beaker, adds distillation to be water-cooled to room
Temperature；Filter, solid-liquid separation, take lyophilization after solid washs 3 times, you can obtain the spherical calcium citrate of self assembly, its SEM schemes such as
Shown in Fig. 2 and 3；Its a diameter of 30-60 micron.Its specific surface area is 25.093m using the test of BET methods2/g。
Embodiment 4
0.8670 gram of CaCl is weighed respectively2, 1.4854 grams of Na3C6H5O7·2H2O, respectively plus 20ml water dissolutioies are in beaker；Will
Na3C6H5O7·2H2O solution adds CaCl2Solution, stirs；The beaker that will be equipped with mixed solution is put in water-bath, water-bath
Temperature is 75 degrees Celsius, and mixing speed is set to 5r/min；Beaker is taken out after 30 minutes, in beaker, adds distillation to be water-cooled to room
Temperature；Filter, solid-liquid separation, take lyophilization after solid washs 3 times, you can obtain the spherical calcium citrate of self assembly, can by SEM figures
Know its a diameter of 30-60 micron.Its specific surface area is 5.132m using the test of BET methods2/g。
Test example 1
0.8670 gram of CaCl is taken respectively2, 1.4854 grams of Na3C6H5O7·2H2O, respectively plus 20ml water dissolutioies are in beaker, will
Na3C6H5O7·2H2O solution adds CaCl20.2g berberine hydrochloride is added stirring in mixed solution equal after stirring by solution
Even, other steps are with embodiment 2.With the release conditions of UV spectrophotometer measuring berberine hydrochloride, drug release patterns are such as
Shown in Fig. 4.As seen from Figure 4：
Release of the medicine in calcium citrate microsphere can be divided into three phases：First stage is 0-30min, and second stage is
30-60min, phase III are 60-90min, and after 90min, medicine substantially completely discharges；Drug release speed in first stage
Degree quickly, releases about 71.5% medicine in 30min；The rate of release of second stage medicine becomes than shallower, the rank
Section only releases about 10.7% medicine；Phase III drug releasing rate is accelerated, and rate of release is high less than the first stage
In second stage, the stage releases about 17.8% medicine.
The drug release patterns are relevant with the unique texture of calcium citrate；Due to medicine carrying microballoonss be by lamellar calcium citrate from
What assembling was formed, the specific surface area of microsphere extexine is big, big with the contact surface of solution, and during so as to starting, drug releasing rate is very
Hurry up；Second stage is probably that the specific surface area of microsphere internal layer is less, and medicine and the solution contact surface of parcel accumulate less so as to discharge
Slow；And with extexine in the solution soak time increase and gradually come off, internal layer is come out so that internal layer bag
The drug releasing rate wrapped up in is accelerated until discharging completely.
The present invention requires that to rate of release medicine is acted on than larger faster, due to the specific surface area of the spherical calcium citrate
Larger, medicine is attached in the performance of lamellar calcium citrate, and medicine is big with environment contact area, thus the rate of release of medicine
It is larger, it is seen then that the spherical calcium citrate of present invention gained can medicine provides a kind of load well faster to need rate of release
Body.
Claims (7)
1. a diameter of 10-100 μm, be 1～80m based on the specific surface area that BET method is determined2The calcium citrate of/g is used as drug release
Carrier prepares the purposes of medicine.
2. purposes according to claim 1, it is characterised in that a diameter of 30～60 μm of the calcium citrate, specific surface
Product is 1～51m2/g。
3. purposes according to claim 1 and 2, it is characterised in that the spherical calcium citrate by lamellar calcium citrate from
Assemble.
4. the purposes according to any one of claims 1 to 3, it is characterised in that the spherical calcium citrate is by preparing as follows
Method is prepared from：Water-soluble Ca salt and water-soluble citrate are added water be uniformly mixed so as to obtain calcium salt and citrate mixing it is water-soluble
Resulting solid-liquid is mixed by the mixed aqueous solution of liquid, calcium salt and citrate in 40～99 DEG C of heated and stirred 2min-30min
Thing solid-liquid separation, wash and be dried to obtain spherical calcium citrate；Wherein, in the mixed aqueous solution of calcium salt and citrate, massage
You compare, 2.5 ︰ 2 of Gai Li ︰ citrates ＞.
5. purposes according to claim 4, it is characterised in that Gai Li ︰ citrate=2.8～3.2 ︰ 2.
6. purposes according to claim 4, it is characterised in that the water-soluble Ca salt is calcium chloride, in calcium nitrate extremely
Few one kind；The water-soluble citrate is trisodium citrate, potassium citrate, at least one in Triammonium citrate.
7. purposes according to claim 5, it is characterised in that the water-soluble Ca salt is calcium chloride, in calcium nitrate extremely
Few one kind；The water-soluble citrate is trisodium citrate, potassium citrate, at least one in Triammonium citrate.
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| CN108218694B (en) * | 2018-01-30 | 2020-12-25 | 日照金禾博源生化有限公司 | Preparation method of superfine calcium citrate |
| CN108853516B (en) * | 2018-07-07 | 2023-01-06 | 成都迈德克科技有限公司 | Functional medicine-carrying calcium citrate |
| CN115572222B (en) * | 2022-08-11 | 2024-05-10 | 山东金禾保健品有限公司 | Preparation method and application of spherical calcium citrate crystal |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073333A (en) * | 1991-12-20 | 1993-06-23 | 卡夫通用食品有限公司 | Aqueous calcium citrate compositions |
| CN101185772A (en) * | 2007-12-12 | 2008-05-28 | 彭磊 | Human body hard tissue filling renovation material containing calcium citrate |
| CN102921036A (en) * | 2012-10-11 | 2013-02-13 | 海南医学院 | Method for preparing marine environment-friendly calcium citrate hard tissue repair material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999001121A1 (en) * | 1997-07-01 | 1999-01-14 | Pfizer Inc. | Sertraline salts and sustained-release dosage forms of sertraline |
| AU2007329373B2 (en) * | 2006-12-04 | 2013-06-20 | Supernus Pharmaceuticals, Inc. | Enhanced immediate release formulations of topiramate |
| CN102334690A (en) * | 2010-07-27 | 2012-02-01 | 河北农业大学 | Method for preparing calcium citrate from oyster shell and scallop shell |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073333A (en) * | 1991-12-20 | 1993-06-23 | 卡夫通用食品有限公司 | Aqueous calcium citrate compositions |
| CN101185772A (en) * | 2007-12-12 | 2008-05-28 | 彭磊 | Human body hard tissue filling renovation material containing calcium citrate |
| CN102921036A (en) * | 2012-10-11 | 2013-02-13 | 海南医学院 | Method for preparing marine environment-friendly calcium citrate hard tissue repair material |
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