CN103142551B - Method for preparing micro-capsule by taking xanthan gum and gelatine as wall materials through complex coacervation method - Google Patents
Method for preparing micro-capsule by taking xanthan gum and gelatine as wall materials through complex coacervation method Download PDFInfo
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Abstract
The invention relates to the technical field of preparation of micro-capsules, in particular to a method for preparing a micro-capsule by taking xanthan gum and gelatine as wall materials through a complex coacervation method. The invention aims to solve the problems of being low in micro-capsule encapsulation efficiency and large in grain diameter prepared by the current method. The preparation method comprises the following steps of: 1, preparing gelatine solution; 2, preparing xanthan gum solution; 3, preparing steady O/W type emulsion, and then adding the xanthan gum solution to obtain mixed solution; 4, adding a curing agent after adjusting pH of the mixed solution; and 5, drying to obtain the micro-capsule. The method disclosed by the invention has the advantages that the encapsulation efficiency can be above 90%; the drug loading capacity can be up to 70% maximally; if being placed below 60 DEG C for 10 days, the micro-capsule is only oxidized by 3-8%; the antioxidant ability is strong; in the event of carrying out an in-vitro drug release test, the whole drug releasing time is 12 hours; the accumulated release rate can be above 90%; the slow-release effect is good; and the method disclosed by the invention is mainly used for preparing the micro-capsule by taking xanthan gum and gelatine as the wall materials through the complex coacervation method.
Description
Technical field
The present invention relates to microcapsule preparing technical field, be specifically related to a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation.
Background technology
Microcapsule technology arises from the thirties in 20th century, and the Wurster of the U.S. has prepared microcapsule with physical method.To 20 century 70s, the technique of microcapsule technology is increasingly mature, and range of application expands gradually, and it was coated and expanded to the numerous areas such as medicine, food, household chemicals, fertilizer, chemical industry without charcoal manifolding from initial medicine today.At present, microcapsule technology develops rapidly abroad, and the U.S. locates leading position to its research always.Approximately there is 60% food to adopt this technology in the U.S..The whole world to the research institution of microcapsule technology from 02 year 2% rise to 06,07 year 22% absolutely prove the extensive attention that microcapsule technology causes in the whole world.The research of China is started late, and has introduced this concept in 80 mid-terms in generation of 20th century, although also have many development in microcapsule technology application aspect, with abroad comparing, China is still in the starting stage, and import microcapsule is still occupied an leading position aborning.
Microcapsule technology is that trace substance is wrapped in the technology in thin polymer film, is the microdisplay package technology of a kind of store solids, liquid, gas.Refer to specifically the various natural or synthetic macromolecular compound continuous films (wall or foreign minister) of a certain goal object (core or interior phase) are coated completely; and it is at all harmless to original chemical property of goal object; then little by little by some outside stimulus or slow releasing function, the function of goal object is presented again in outside, or rely on the shielding action of cyst wall to play the effect of protection core.
The size of microcapsule is in nanometer between hundreds of micron and have special nucleus shell structure, and its hollow space can hold a large amount of guest molecules or the object of large-size, the feature such as have that density is low, specific surface area large, good stability, surperficial penetrating power are strong.In recent years, microcapsule technology is used widely in fields such as biomedical engineering, chemical industry, medicine, spice, cosmetics, pressure-sensitive carbon paper and liquid crystal.No matter hydrophilic or lipophilicity substance, most gas, liquid, solid can be encapsulated.Microencapsulation have improve core physical property, protect core, prevent core inactivation, attenuation, minimizing reacting to each other and regulating the effects such as Release of core material between composition when composite.
Complex coacervation is prepared the process that microcapsule is the macromolecular compound formation condensation product of two kinds of oppositely chargeds in solution.By changing the various conditions of system as pH value, temperature or concentration of aqueous solution cause reducing of system surfaces tension force, cause core to be wrapped to form mutually microcapsule by coacervation.
Through retrieval, the patent that existing China Patent Publication No. CN101053810A, name are called " preparation method of high molecular nanometer capsule " discloses the micro nanometer capsule preparation method that can be applied to conventional Ultrasound radiography and molecular imaging, in this patent, gelatin is to make stabilizing agent instead of introduce as wall material, and there is no the objective evaluation such as drug loading, envelop rate index.Separately having the people's such as Wang Yufeng document " complex coacervation is prepared rhizome of chuanxiong and return the research of volatile oil microencapsulation technique " is taking gelatin, arabic gum as wall material, Rhizoma Chuanxiong, Radix Angelicae Sinensis volatile oil are core, adopt complex coacervation to prepare the microcapsule of mean diameter for (297.5 ± 82.8) μ m, with Yield of Mitoxantrone as evaluation index, the highest envelop rate is only 83.5%, the preferred microcapsule preparation process condition of orthogonal design, the microencapsulation rate of preparation is low and particle diameter is large, has no at present the method for preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation.
Summary of the invention
The present invention will solve the low and large problem of particle diameter of microencapsulation rate prepared by existing method, and a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation is provided.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of the present invention comprises the following steps:
One, gelatin is added to the water, soaks after 20min～30min, heating is dissolved it, obtains the gelatin solution that concentration is 0.05g/mL～0.45g/mL, leaves standstill 6h～8h;
Two, xanthan gum is added to the water, soaks after 20min～30min, heating is dissolved it, obtains the xanthan gum solution that concentration is 0.001g/mL～0.05g/mL, leaves standstill 6h～8h;
Three, in the gelatin solution of preparing in step 1, add core, high shear 20s～40s, obtains stable O/W type Emulsion, then drip wherein the xanthan gum solution of preparing in step 2, be under the condition of 50～60 DEG C in temperature, constant temperature stirs 15min～25min, obtains mixed liquor; Wherein in the gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the mass ratio of xanthan gum is 1: (0.2～2.5); In gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the ratio of the quality sum of xanthan gum and the quality of the core described in step 3 is 1: (0.4～2.3);
The pH value of the mixed liquor four, step 3 being obtained is adjusted to 3.5～4.5, obtains pH and be 3.5～4.5 mixed liquor, then adds firming agent, after reaction 30min～120min, obtains microcapsule suspension; In the mixed liquor that wherein pH described in the firming agent described in step 4 and step 4 is 3.5～4.5, the mass ratio of gelatin is 1: (0.5～2.0);
Five, the microcapsule suspension that step 4 obtained is dry, obtains the microcapsule taking xanthan gum and gelatin as wall material.
The method of the microcapsule that the present invention is prepared by complex coacervation taking xanthan gum and gelatin as wall material, taking water-soluble high-molecular compound as natural food material, use safety, stable in properties, make the macromolecular compound in solution form polymer by changing the pH value of system, the pH value of system simultaneously, the variation of temperature or concentration of aqueous solution causes that emulsion systems is capillary to be reduced, thereby core is wrapped up by the condensed phase of wall material, reach the protection to core medicine, isolated or reduced contacting of core medicine and oxygen, prevent core drug inactivation, greatly improve the storage time of core medicine.Technological operation of the present invention is simple, preparation process mild condition, equipment needed thereby is simple, adjuvant used is inexpensive, be easy to get, solvent for use is water, nontoxic, realize the zero-emission of producing, the microcapsule diameter distribution homogeneous of preparation, narrow diameter distribution, microcapsule diameter can reach 0.5 μ m～1 μ m, surface compact, good heat resistance, specific surface area is large, there is good surperficial penetrating power, and gained powder has good mobility, and be difficult for the moisture absorption, envelop rate can reach more than 90%, drug loading reaches as high as 70%, at 60 DEG C, place 10 days only oxidized 3%～8%, oxidation resistance is strong, carry out the test of vitro drug release degree, the time of release overall process is 12 hours, preparation can reach more than 90%, had good sustained release effect, can also be by regulating and controlling microcapsule size and core content to reach various objects, easily realize large-scale production.
Brief description of the drawings
Fig. 1 is Rhizoma Chuanxiong oil microcapsule and the Rhizoma Chuanxiong oil crude drug antioxidation Experimental Comparison curve chart that embodiment 1 obtains; Wherein ■ is the Rhizoma Chuanxiong oil microcapsule that embodiment 1 obtains, ◆ be Rhizoma Chuanxiong oil crude drug.
Fig. 2 is the vitro release test rate of releasing drug curve chart of the Rhizoma Chuanxiong oil microcapsule that obtains of embodiment 1.
Detailed description of the invention
Detailed description of the invention one: a kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of present embodiment comprises the following steps:
One, gelatin is added to the water, soaks after 20min～30min, heating is dissolved it, obtains the gelatin solution that concentration is 0.05g/mL～0.45g/mL, leaves standstill 6h～8h;
Two, xanthan gum is added to the water, soaks after 20min～30min, heating is dissolved it, obtains the xanthan gum solution that concentration is 0.001g/mL～0.05g/mL, leaves standstill 6h～8h;
Three, in the gelatin solution of preparing in step 1, add core, high shear 20s～40s, obtains stable O/W type Emulsion, then drip wherein the xanthan gum solution of preparing in step 2, be under the condition of 50～60 DEG C in temperature, constant temperature stirs 15min～25min, obtains mixed liquor; Wherein in the gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the mass ratio of xanthan gum is 1: (0.2～2.5); In gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the ratio of the quality sum of xanthan gum and the quality of the core described in step 3 is 1: (0.4～2.3);
The pH value of the mixed liquor four, step 3 being obtained is adjusted to 3.5～4.5, obtains pH and be 3.5～4.5 mixed liquor, then adds firming agent, after reaction 30min～120min, obtains microcapsule suspension; In the mixed liquor that wherein pH described in the firming agent described in step 4 and step 4 is 3.5～4.5, the mass ratio of gelatin is 1: (0.5～2.0);
Five, the microcapsule suspension that step 4 obtained is dry, obtains the microcapsule taking xanthan gum and gelatin as wall material.
The method of the microcapsule that present embodiment is prepared by complex coacervation taking xanthan gum and gelatin as wall material, taking water-soluble high-molecular compound as natural food material, use safety, stable in properties, make the macromolecular compound in solution form polymer by changing the pH value of system, the pH value of system simultaneously, the variation of temperature or concentration of aqueous solution causes that emulsion systems is capillary to be reduced, thereby core is wrapped up by the condensed phase of wall material, reach the protection to core medicine, isolated or reduced contacting of core medicine and oxygen, prevent core drug inactivation, greatly improve the storage time of core medicine.Present embodiment technological operation is simple, preparation process mild condition, equipment needed thereby is simple, adjuvant used is inexpensive, be easy to get, solvent for use is water, nontoxic, realize the zero-emission of producing, the microcapsule diameter distribution homogeneous of preparation, narrow diameter distribution, microcapsule diameter can reach 0.5 μ m～1 μ m, surface compact, good heat resistance, there is good surperficial penetrating power, and gained powder has good mobility, and be difficult for the moisture absorption, envelop rate can reach more than 90%, drug loading reaches as high as 70%, at 60 DEG C, place 10 days only oxidized 3%～8%, oxidation resistance is strong, carry out the test of vitro drug release degree, the time of release overall process is 12 hours, preparation can reach more than 90%, had good sustained release effect, can also be by regulating and controlling microcapsule size and core content to reach various objects, easily realize large-scale production.
Detailed description of the invention two: present embodiment is different from detailed description of the invention one: obtain the gelatin solution that concentration is 0.25g/mL in step 1, other steps and parameter are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is different from detailed description of the invention one or two: obtain the xanthan gum solution that concentration is 0.01g/mL in step 2, other steps and parameter are identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment is different from one of detailed description of the invention one to three: in step 3, core is oiliness medicine, oil-soluble medicine or solid drugs, other steps and parameter are identical with one of detailed description of the invention one to three.
Detailed description of the invention five: present embodiment is different from one of detailed description of the invention one to four: in step 3,, under temperature is the condition of 55 DEG C, constant temperature stirs 20min, and other steps and parameter are identical with one of detailed description of the invention one to four.
Detailed description of the invention six: present embodiment is different from one of detailed description of the invention one to five: in the gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the ratio of the quality sum of xanthan gum and the quality of the core described in step 3 is 1: (1～2), other steps and parameter are identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: present embodiment is different from one of detailed description of the invention one to six: the pH value of the mixed liquor in step 4, step 3 being obtained is adjusted to 4, obtain pH and be 4 mixed liquor, other steps and parameter are identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment is different from one of detailed description of the invention one to seven: the firming agent described in step 4 is glutaraldehyde, TG enzyme, tannin or sodium tripolyphosphate, and other steps and parameter are identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: present embodiment is different from one of detailed description of the invention one to eight: in the mixed liquor that the pH described in the firming agent described in step 4 and step 4 is 3.5～4.5, the mass ratio of gelatin is 1: (1～1.5), other steps and parameter are identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment is different from one of detailed description of the invention one to nine: the microcapsule suspension that the dry employing described in step 5 obtains step 4 first filters, then filtrate is dry, or the microcapsule suspension Direct spraying that step 4 is obtained is dry, and other steps and parameter are identical with one of detailed description of the invention one to nine.
By following verification experimental verification beneficial effect of the present invention:
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 1, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 7.5g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The Rhizoma Chuanxiong oil microcapsule good fluidity that the present embodiment obtains, uniform particle diameter, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 93.5%.
Test one, according to according to second annex XI XC of Pharmacopoeia of People's Republic of China version in 2000, medicine stability test guideline, Rhizoma Chuanxiong oil microcapsule and Rhizoma Chuanxiong oil that embodiment 1 is obtained are positioned over respectively in electro-heating standing-temperature cultivator, be under 60 DEG C of conditions in temperature, place 10 days, carry out the contrast test of oxidation stability, result as shown in Figure 1, wherein ■ is that the present embodiment obtains Rhizoma Chuanxiong oil microcapsule, ◆ be Rhizoma Chuanxiong oil crude drug.As can be seen from Figure 1 the Rhizoma Chuanxiong oil microcapsule of the present embodiment at 60 DEG C, place 10 days only oxidized 8%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of embodiment 1 is good as can be seen here.
Test two, according to second annex XI XD of Pharmacopoeia of People's Republic of China version in 2000, slow release, controlled release preparation guideline, adopt the intelligent dissolving-out tester that model is ZRS-8G, embodiment 1 is obtained to Rhizoma Chuanxiong oil microcapsule and carry out the test of vitro drug release degree, result as shown in Figure 2, the time of release overall process is 12 hours, and preparation is 93.2%, and the Rhizoma Chuanxiong oil microcapsule of visible embodiment 1 has good slow release effect.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 2, the present embodiment comprises the following steps:
One, 7.5g gelatin is joined in the distilled water of 30ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 10g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 7.5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 91.5%.
Adopt test one instrument and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained and Rhizoma Chuanxiong oil crude drug carry out the contrast test of oxidation stability, the Rhizoma Chuanxiong oil microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 5%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 95.8%, and the Rhizoma Chuanxiong oil microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 3, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 50ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.1g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 50ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.05g/mL, standing 8h; Three, in the gelatin solution that is 0.1g/mL to the concentration of preparing in step 1, add 7.5g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.05g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 94.3%.
Adopt test one instrument and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained and Rhizoma Chuanxiong oil crude drug carry out the contrast test of oxidation stability, the Rhizoma Chuanxiong oil microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 3%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 93.4%, and the Rhizoma Chuanxiong oil microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 4, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 7.5g paeonol, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains paeonol microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 93.8%.
Adopt test one instrument and method, the paeonol microcapsule that the present embodiment is obtained and paeonol crude drug, carry out the contrast test of oxidation stability, the paeonol microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 5%, and paeonol crude drug is under similarity condition oxidized 98%.The oxidation resistance of the paeonol microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the paeonol microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 96.9%, and the paeonol microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 5, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 17.5g eugenol, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains eugenol microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 70%, envelop rate is 92.5%.
Adopt test one instrument and method, the eugenol microcapsule that the present embodiment is obtained and eugenol crude drug, carry out the contrast test of oxidation stability, the eugenol microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 8%, and eugenol crude drug is under similarity condition oxidized 96%.The oxidation resistance of the eugenol microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the eugenol microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 95.8%, and the eugenol microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 6, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 17.5g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 95.0%.
Adopt test one instrument and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained and Rhizoma Chuanxiong oil crude drug, carry out the contrast test of oxidation stability, the Rhizoma Chuanxiong oil microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 7%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 97.9%, and the Rhizoma Chuanxiong oil microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 7, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 7.5g Radix Angelicae Sinensis oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 3.5, then add 5g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 94.5%.
Adopt test one instrument and method, the Radix Angelicae Sinensis oil microcapsule that the present embodiment is obtained and Radix Angelicae Sinensis oil crude drug, carry out the contrast test of oxidation stability, the microcapsule of the Radix Angelicae Sinensis oil wall material that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 4%, and Radix Angelicae Sinensis oil crude drug is under similarity condition oxidized 92%.The oxidation resistance of the Radix Angelicae Sinensis oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Radix Angelicae Sinensis oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 94.2%, and the Radix Angelicae Sinensis oil microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 8, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 7.5g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 10g glutaraldehyde, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 93.5%.
Adopt test one instrument and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained and Rhizoma Chuanxiong oil crude drug, carry out the contrast test of oxidation stability, the Rhizoma Chuanxiong oil microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 5%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 96.5%, and the Rhizoma Chuanxiong oil microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 9, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 7.5g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5gTG enzyme, after reaction 40min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, uniform particle diameter, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 92.5%.
Adopt test one instrument and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained and Rhizoma Chuanxiong oil crude drug, carry out the contrast test of oxidation stability, the Rhizoma Chuanxiong oil microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 3%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 91.9%, and the Rhizoma Chuanxiong oil microcapsule of the present embodiment has good slow release effect as can be seen here.
A kind of method of preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin of embodiment 10, the present embodiment comprises the following steps:
One, 5g gelatin is joined in the distilled water of 20ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the gelatin that concentration is 0.25g/mL, standing 8h; Two, 2.5g xanthan gum is joined in the distilled water of 250ml, soak after 20min, in temperature is the water-bath of 55 DEG C, heat it is dissolved, obtain the xanthan gum solution that concentration is 0.01g/mL, standing 8h; Three, in the gelatin solution that is 0.25g/mL to the concentration of preparing in step 1, add 7.5g Rhizoma Chuanxiong oil, emulsifying 30s under high shear, obtain stable O/W type Emulsion, then the xanthan gum solution that to drip wherein the concentration prepared in step 2 be 0.01g/mL, be under the condition of 55 DEG C in temperature, constant temperature stirs 20min, obtains mixed liquor; Four, in the mixed liquor obtaining to step 3, to add mass concentration be 0.5% vinegar acid for adjusting pH value to pH be 4, then add 5g glutaraldehyde, after reaction 120min, obtain microcapsule suspension; Five, microcapsule suspension step 4 being obtained is sprayed dry, obtains Rhizoma Chuanxiong oil microcapsule.
The microcapsule good fluidity of the present embodiment, uniform particle diameter, smooth outer surface, softgel shell densification, drug loading is 50%, envelop rate is 91.3%.
Adopt test one instrument and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained and Rhizoma Chuanxiong oil crude drug, carry out the contrast test of oxidation stability, the Rhizoma Chuanxiong oil microcapsule that the present embodiment obtains at 60 DEG C, place 10 days only oxidized 6%, and Rhizoma Chuanxiong oil crude drug is under similarity condition oxidized 97%.The oxidation resistance of the Rhizoma Chuanxiong oil microcapsule of the present embodiment is good as can be seen here.
Adopt test two instruments and method, the Rhizoma Chuanxiong oil microcapsule that the present embodiment is obtained carries out the test of vitro drug release degree, the time of release overall process is 12 hours, and preparation is 98.6%, and the Rhizoma Chuanxiong oil microcapsule of the present embodiment has good slow release effect as can be seen here.
Claims (9)
1. prepare a method for microcapsule taking xanthan gum and gelatin as wall material complex coacervation, it is characterized in that the method for preparing microcapsule as wall material complex coacervation taking xanthan gum and gelatin comprises the following steps:
One, gelatin is added to the water, soaks after 20min～30min, heating is dissolved it, obtains the gelatin solution that concentration is 0.05g/mL～0.45g/mL, leaves standstill 6h～8h;
Two, xanthan gum is added to the water, soaks after 20min～30min, heating is dissolved it, obtains the xanthan gum solution that concentration is 0.001g/mL～0.05g/mL, leaves standstill 6h～8h;
Three, in the gelatin solution of preparing in step 1, add core, high shear 20s～40s, obtains stable O/W type Emulsion, then drip wherein the xanthan gum solution of preparing in step 2, be under the condition of 50～60 DEG C in temperature, constant temperature stirs 15min～25min, obtains mixed liquor; Wherein in the gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the mass ratio of xanthan gum is 1: (0.2～2.5); In gelatin solution described in step 3, in the xanthan gum solution described in quality and the step 3 of gelatin, the ratio of the quality sum of xanthan gum and the quality of the core described in step 3 is 1: (0.4～2.3);
The pH value of the mixed liquor four, step 3 being obtained is adjusted to 4, obtains pH and be 4 mixed liquor, then adds firming agent, after reaction 30min～120min, obtains microcapsule suspension; In the mixed liquor that wherein pH described in the firming agent described in step 4 and step 4 is 4, the mass ratio of gelatin is 1: (0.5～2.0);
Five, the microcapsule suspension that step 4 obtained is dry, obtains the microcapsule taking xanthan gum and gelatin as wall material.
2. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 1, is characterized in that obtaining in step 1 the gelatin solution that concentration is 0.25g/mL.
3. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 1 and 2, is characterized in that obtaining in step 2 the xanthan gum solution that concentration is 0.01g/mL.
4. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 3, is characterized in that in step 3, core is oiliness medicine, oil-soluble medicine or solid drugs.
5. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 3, is characterized in that in step 3 that constant temperature stirs 20min under temperature is the condition of 55 DEG C.
6. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 3, is characterized in that in the xanthan gum solution described in quality and the step 3 of gelatin in the gelatin solution described in step 3, the ratio of the quality sum of xanthan gum and the quality of the core described in step 3 is 1: (1～2).
7. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 3, is characterized in that the firming agent described in step 4 is glutaraldehyde, TG enzyme, tannin or sodium tripolyphosphate.
8. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 3, is characterized in that the pH described in the firming agent described in step 4 and step 4 is that in 4 mixed liquor, the mass ratio of gelatin is 1: (1～1.5).
9. a kind of method of preparing microcapsule taking xanthan gum and gelatin as wall material complex coacervation according to claim 3, it is characterized in that the microcapsule suspension that the dry employing described in step 5 obtains step 4 first filters, then filtrate is dry, or the microcapsule suspension Direct spraying that step 4 is obtained is dry.
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| CN106721618A (en) * | 2016-12-05 | 2017-05-31 | 陈庆功 | A kind of nutrition crucian carp feed in a balanced way |
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| CN114711320A (en) * | 2022-04-20 | 2022-07-08 | 深圳靓维食品有限公司 | Preparation method of sugar-free soft sweets with eye protection function |
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| 王玉凤等.复凝聚法制备芎归挥发油微型胶囊工艺的研究.《北京中医药》.2008,第27卷(第9期),第731－732页. |
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