CN108498478A - A kind of preparation method of starch base hard capsule - Google Patents
A kind of preparation method of starch base hard capsule Download PDFInfo
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- CN108498478A CN108498478A CN201810286402.0A CN201810286402A CN108498478A CN 108498478 A CN108498478 A CN 108498478A CN 201810286402 A CN201810286402 A CN 201810286402A CN 108498478 A CN108498478 A CN 108498478A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
- C08B31/10—Alkyl or cycloalkyl ethers
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- 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
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
Abstract
The invention belongs to technical field of medicine preparation, specifically disclose a kind of preparation method of starch base hard capsule.The preparation method includes starch acidolysis, etherificate, colloidal sol, heat preservation, defoams, dips in gum forming, drying and other steps.The present invention is using acidolysis and is etherified composite modified processing starch, reduces the viscosity of starch, while improving the filming performance of starch；It for 80% high amylose starches is matrix to use amylose content, and modified starch is reinforced phase, and the technique for passing through traditional dip mold prepares starch base hard capsule.Not only have many advantages, such as that transparency is high by the starch base hard capsule prepared by the method for the present invention, show that smooth, folding resistance is good, disintegration time limited is short, also simplifies production technology, be suitble to large-scale promotion application.
Description
Technical field
The present invention relates to technical field of medicine preparation, and in particular, to a kind of preparation method of starch base hard capsule.
Background technology
Capsule, which is generally used for package, directly to be contacted with esophagus, and the drug of calving disaggregation again is needed in stomach or enteron aisle.
Most of medicinal or health food hard capsule is made of gelatin at present, and gelatin still has one in pharmaceutical characteristic and secure context
Fixed problem.On the one hand, gelatin comes from the skin or bone of animal, through acid or alkali process, boils and obtains.In its production process, no
It is evitable to have animal protein residual, it is easy and content drug crosslinks reaction and takes viruliferous risk, to lead
The adverse consequences such as cause drug rotten.On the other hand, the gelatin of animal origin, for vegetarian and hold Islam, still
The personage of the religious beliefs such as too is unacceptable.In addition, for the crowd of allergic constitution, and intake gelatin system should be avoided
Product.Therefore, finding the substitute of gelatine capsule seems particularly important.
Starch is plant origin, derives from a wealth of sources and price is very cheap, has preferable filming performance, is prepared with it hollow
Capsule has prodigious attraction, but due to being easily formed very strong hydrogen bond between starch molecule, and it is frangible brittle to prepare starch film, difficult
The Capsules of high, the resistance to filling of intensity are made.In the existing technique for preparing starch hard capsule using traditional dip mold method
In, maximum difficulty is exactly that starch solution viscosity is excessively high, is difficult to control thickness.Therefore, suitable modified starch materials are found, and
The phase transformation of the rheology and filming performance and starch of starch material in process is studied to meet the equipment of traditional gelatin as possible
It is one of current urgent need to solve the problem with technique.
Invention content
The purpose of the invention is to overcome the above-mentioned deficiency of the prior art, a kind of preparation side of starch base hard capsule is provided
Method using acidolysis and is etherified composite modified processing starch, reduces the viscosity of starch, while improving the filming performance of starch；Using
The high amylose starches that amylose content is 80% is matrix, and modified starch is reinforced phase, passes through the technique system of traditional dip mold
Standby starch base hard capsule.
Another object of the present invention is to provide the starch base hard capsules that the above method is prepared to prepare drug, health care
Application in product and functional food.
To achieve the goals above, the present invention is achieved by following scheme：
A kind of preparation method of starch base hard capsule, includes the following steps：
S1. take appropriate amount of starch that starch is configured to the starch milk of content of starch 40% with the hydrochloric acid solution of a concentration of 0.14mol/L,
It is placed in 35~40 DEG C, acidolysis 6 under the conditions of 200rpm~for 24 hours；Use the NaOH solution that mass fraction is 5% by the pH tune of starch milk again
To 5.5；Liquid is discarded supernatant after centrifugation, two volumes water centrifuge washing is added 3 times, in 40~45 DEG C of drying 10~12h of reaction, is obtained
Acidified starch；
S2. take acidified starch obtained by S1, the starch milk of content of starch 20% be configured to water, be added mass fraction be 10% it is anhydrous
Metabisulfite solution, stir and heating water bath to 40 DEG C reaction 10min；Mass fraction is added while stirring will for 5% NaOH solution
The pH of reaction system is adjusted to 10.5 or more, rapidly join volume fraction be 10~30% propylene oxide, be placed in closed container in
35~40 DEG C, etherification reaction 21 under the conditions of 200rpm~for 24 hours；Use the dilute hydrochloric acid that mass fraction is 10% by the pH tune of starch milk again
To 5.5；Liquid is discarded supernatant after centrifugation, two volumes water centrifuge washing is added 3 times, in 40~45 DEG C of drying 10~12h of reaction, is obtained
Modified starch；
S3. the starch solution that configuration quality score is 10~20%, the starch are grouped as by each group of following mass percent：
Modified starch 30~60% and high amylose starches 40~70%；Starch solution is stirred into colloidal sol 40min, heat preservation defoaming in 93~97 DEG C
After dip in glue, after 35~38 DEG C of dry 6~9h demoulding to get starch base hard capsule.
In the technique for preparing starch hard capsule using traditional dip mold method, maximum difficulty is exactly starch solution viscosity
It is excessively high, it is difficult to control thickness.And the present invention can reduce the viscosity of starch by acidolysis, and the shallow lake that concentration is higher, easily forms a film can be made
Paste mixing liquid；But the easy retrogradation of acidified starch, viscosity stability are relatively low, and propylene oxide is added and carries out the converted starch after etherification reaction
Gelatinization point is low, and starch molecule can be disperseed and be dissolved well after heating, forms the starch of mobility and viscosity stabilization
Paste, thus gelatinized corn starch formed thin-film transparent, flexible, smooth, folding resistance is good.Therefore, starch is composite modified through acidolysis, etherificate etc.
Afterwards, the performance of two kinds of modified starches can be optimized, obtains better gelling ability and mechanical strength, is close to the property of gelatin
Matter.It for 80% high amylose starches is matrix to use amylose content, and modified starch is reinforced phase, not only may be used by self-reinforcing
To improve the mechanical property of capsule, and their biocompatibility is not interfered with.These three key process technologies solve
Starch high, film forming difference problem as capsule viscosity, improves the quality of starch capsule.
Preferably, starch described in S1 is cornstarch, tapioca, potato starch any one or more of.
Preferably, high amylose starches described in S3 is amylomaize G80, the higher para arrowroot of amylose content
Powder or potato starch any one or more of.
It is highly preferred that starch described in S1 is cornstarch, high amylose starches described in S3 is amylomaize
G80。
The present inventor has found in the exploration for the technique for preparing starch hard capsule to traditional dip mold method, sour type
And dosage, the concentration of alkali, the selection of epoxides, the proportioning of matrix and reinforced phase, the temperature and time of acidolysis reaction, etherificate are anti-
The preparation parameters such as the temperature and time answered to the transparency of finally obtained starch base hard capsule, toughness, friability, elasticity and
Disintegration time limited etc. all has a significant impact.If the too low reaction rate of reaction temperature is excessively slow, the too high starch of temperature is easy gelatinization.The present invention
By the preferred of this series of conditions, most preferred preparation parameter is finally obtained, is prepared that transparency is high, it is smooth, resistance to show
The starch base hard capsule that folding endurance is good, disintegration time limited is short.
Preferably, the reaction temperature of acidolysis described in S1 is 40 DEG C, reaction time 12h.
Preferably, the volume fraction of propylene oxide described in S2 is 20%.
Preferably, the reaction temperature being etherified described in S2 is 40 DEG C, reaction time 22h.
Preferably, centrifugal rotational speed described in S1 and S2 is 5000r/min, centrifugation time 10min.
Preferably, starch described in S3 is grouped as by each group of following mass percent：Modified starch 40% and high straight chain form sediment
Powder 60%.
Preferably, the temperature of colloidal sol described in S3 is 95 DEG C.
Preferably, temperature dry described in S3 is 35 DEG C, time 6h.
The starch base hard capsule being prepared by the above method meets relative national standards, has transparency height, shows light
Sliding, the advantages that folding resistance is good, disintegration time limited is short.Therefore, it is hard that the starch base that the method is prepared is also claimed in the present invention
Application of the capsule in preparing drug, health products and functional food.
Compared with prior art, the invention has the advantages that：
Method provided by the present invention is using acidolysis and is etherified composite modified processing starch, reduces the viscosity of starch, improves simultaneously
The filming performance of starch；It for 80% high amylose starches is matrix to use amylose content, and modified starch is reinforced phase, is passed through
The technique of traditional dip mold prepares starch base hard capsule.Not only had by the starch base hard capsule prepared by the method for the present invention saturating
Lightness is high, shows the advantages that smooth, folding resistance is good, disintegration time limited is short, also simplifies production technology, saves production cost, is suitble to
Large-scale promotion application.
Specific implementation mode
The present invention is made with specific embodiment below and further being elaborated, the embodiment is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.Test method used in following embodiments is routine unless otherwise specified
Method；Used material, reagent etc., unless otherwise specified, for the reagent and material commercially obtained.
Embodiment 1
The present embodiment provides a kind of preparation methods of starch base hard capsule, include the following steps：
1, a certain amount of cornstarch is accurately weighed, is placed in stainless steel allocates container, with the hydrochloric acid solution of a concentration of 0.14mol/L
It configures starch to the starch milk of content of starch 40%, is placed in 35 DEG C, carries out acidolysis 11h in the constant-temperature shaking incubator of 200rpm.
After acidolysis, the pH value of starch milk is adjusted to 5.5 by the NaOH solution for being 5% with mass fraction.First discarded with centrifuge
Clear liquid, it is 5000r/min then to use the distilled water centrifuge washing 3 times of two volumes, setting centrifuge speed again, and centrifugation time is
10min, later in baking oven（40~45 DEG C）Middle reaction 10h, obtains acidified starch.
2, step 1 gained acidified starch is taken, the starch milk of content of starch 20% is made into distilled water, pours into stainless steel reaction
In device, the anhydrous slufuric acid sodium solution that mass fraction is 10%, stirring and heating water bath is added to 40 DEG C of isothermal reaction 10min；While stirring
It mixes the NaOH that side addition mass fraction is 5% and the pH of reaction system is adjusted to 10.5 or more, be then quickly added into a certain amount of volume
The propylene oxide that score is 10%, is placed in closed container the etherification reaction 21h under the conditions of 35 DEG C, 200rpm.After reaction,
The pH of starch milk is adjusted to 5.5 by the dilute hydrochloric acid for being 10% with mass fraction.Liquid first is discarded supernatant with centrifuge, is then used again
The distilled water centrifuge washing of two volumes 3 times, setting centrifuge speed are 5000r/min, centrifugation time 10min, Zhi Hou
Baking oven（40~45 DEG C）Middle reaction 10h, obtains modified starch.
3, the starch solution that configuration quality score is 10~20%, the starch are grouped by each group of following mass percent
At：Modified starch 30% and amylomaize G80 70%；Starch solution is put into 93 DEG C of thermostat water baths and stirs colloidal sol
40min dips in glue after heat preservation defoaming, and demoulding is to get starch base hard capsule after 35 DEG C of dry 8h, and meets the related mark of country
It is accurate.
Embodiment 2
The present embodiment provides a kind of preparation methods of starch base hard capsule, include the following steps：
1, a certain amount of cornstarch is accurately weighed, is placed in stainless steel allocates container, with the hydrochloric acid solution of a concentration of 0.14mol/L
It configures starch to the starch milk of content of starch 40%, is placed in 37 DEG C, carries out acidolysis 18h in the constant-temperature shaking incubator of 200rpm.
After acidolysis, the pH value of starch milk is adjusted to 5.5 by the NaOH solution for being 5% with mass fraction.First discarded with centrifuge
Clear liquid, it is 5000r/min then to use the distilled water centrifuge washing 3 times of two volumes, setting centrifuge speed again, and centrifugation time is
10min, later in baking oven（40~45 DEG C）Middle reaction 11h, obtains acidified starch.
2, step 1 gained acidified starch is taken, the starch milk of content of starch 20% is made into distilled water, pours into stainless steel reaction
In device, the anhydrous slufuric acid sodium solution that mass fraction is 10%, stirring and heating water bath is added to 40 DEG C of isothermal reaction 10min；While stirring
It mixes the NaOH that side addition mass fraction is 5% and the pH of reaction system is adjusted to 10.5 or more, be then quickly added into a certain amount of volume
The propylene oxide that score is 30% is placed in closed container under the conditions of 37 DEG C, 200rpm etherification reaction for 24 hours.After reaction,
The pH of starch milk is adjusted to 5.5 by the dilute hydrochloric acid for being 10% with mass fraction.Liquid first is discarded supernatant with centrifuge, is then used again
The distilled water centrifuge washing of two volumes 3 times, setting centrifuge speed are 5000r/min, centrifugation time 10min, Zhi Hou
Baking oven（40~45 DEG C）Middle reaction 11h, obtains modified starch.
3, the starch solution that configuration quality score is 10~20%, the starch are grouped by each group of following mass percent
At：Modified starch 50% and amylomaize G80 50%；Starch solution is put into 97 DEG C of thermostat water baths and stirs colloidal sol
40min dips in glue after heat preservation defoaming, and demoulding is to get starch base hard capsule after 38 DEG C of dry 9h, and meets the related mark of country
It is accurate.
Embodiment 3
The present embodiment provides a kind of preparation methods of starch base hard capsule, include the following steps：
1, a certain amount of cornstarch is accurately weighed, is placed in stainless steel allocates container, with the hydrochloric acid solution of a concentration of 0.14mol/L
It configures starch to the starch milk of content of starch 40%, is placed in 40 DEG C, carries out acidolysis 12h in the constant-temperature shaking incubator of 200rpm.
After acidolysis, the pH value of starch milk is adjusted to 5.5 by the NaOH solution for being 5% with mass fraction.First discarded with centrifuge
Clear liquid, it is 5000r/min then to use the distilled water centrifuge washing 3 times of two volumes, setting centrifuge speed again, and centrifugation time is
10min, later in baking oven（40~45 DEG C）Middle reaction 12h, obtains acidified starch.
2, step 1 gained acidified starch is taken, the starch milk of content of starch 20% is made into distilled water, pours into stainless steel reaction
In device, the anhydrous slufuric acid sodium solution that mass fraction is 10%, stirring and heating water bath is added to 40 DEG C of isothermal reaction 10min；While stirring
It mixes the NaOH that side addition mass fraction is 5% and the pH of reaction system is adjusted to 10.5 or more, be then quickly added into a certain amount of volume
The propylene oxide that score is 20%, is placed in closed container the etherification reaction 22h under the conditions of 40 DEG C, 200rpm.After reaction,
The pH of starch milk is adjusted to 5.5 by the dilute hydrochloric acid for being 10% with mass fraction.Liquid first is discarded supernatant with centrifuge, is then used again
The distilled water centrifuge washing of two volumes 3 times, setting centrifuge speed are 5000r/min, centrifugation time 10min, Zhi Hou
Baking oven（40~45 DEG C）Middle reaction 12h, obtains modified starch.
3, the starch solution that configuration quality score is 10~20%, the starch are grouped by each group of following mass percent
At：Modified starch 40% and amylomaize G80 60%；Starch solution is put into 95 DEG C of thermostat water baths and stirs colloidal sol
40min dips in glue after heat preservation defoaming, and demoulding is to get starch base hard capsule after 35 DEG C of dry 6h, and meets the related mark of country
It is accurate.
Performance evaluation
The starch base hard capsule that Example 1~3 is prepared carries out performance detection, the results are shown in Table 1.
The investigation result of 1 Examples 1 to 3 starch base hard capsule of table
| Appearance character | Friability | Disintegration time limited | |
| Embodiment 1 | Relatively transparent, surface is smooth | 3 | 10min |
| Embodiment 2 | Transparency is high, and surface is smooth | 2 | 9min |
| Embodiment 3 | Transparency is high, and surface is smooth | 0 | 8min |
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects model to the present invention
The limitation enclosed can also be made other on the basis of above description and thinking for those of ordinary skill in the art
Various forms of variations or variation, there is no necessity and possibility to exhaust all the enbodiments.All spirit in the present invention
With within principle made by all any modification, equivalent and improvement etc., should be included in the protection domain of the claims in the present invention
Within.
Claims (10)
1. a kind of preparation method of starch base hard capsule, which is characterized in that include the following steps：
S1. take appropriate amount of starch that starch is configured to the starch milk of content of starch 40% with the hydrochloric acid solution of a concentration of 0.14mol/L,
It is placed in 35~40 DEG C, acidolysis 6 under the conditions of 200rpm~for 24 hours；Use the NaOH solution that mass fraction is 5% by the pH tune of starch milk again
To 5.5；Liquid is discarded supernatant after centrifugation, two volumes water centrifuge washing is added 3 times, in 40~45 DEG C of drying 10~12h of reaction, is obtained
Acidified starch；
S2. take acidified starch obtained by S1, the starch milk of content of starch 20% be configured to water, be added mass fraction be 10% it is anhydrous
Metabisulfite solution, stir and heating water bath to 40 DEG C reaction 10min；Mass fraction is added while stirring will for 5% NaOH solution
The pH of reaction system is adjusted to 10.5 or more, rapidly join volume fraction be 10~30% propylene oxide, be placed in closed container in
35~40 DEG C, etherification reaction 21 under the conditions of 200rpm~for 24 hours；Use the dilute hydrochloric acid that mass fraction is 10% by the pH tune of starch milk again
To 5.5；Liquid is discarded supernatant after centrifugation, two volumes water centrifuge washing is added 3 times, in 40~45 DEG C of drying 10~12h of reaction, is obtained
Modified starch；
S3. the starch solution that configuration quality score is 10~20%, the starch are grouped as by each group of following mass percent：
Modified starch 30~60% and high amylose starches 40~70%；Starch solution is stirred into colloidal sol 40min, heat preservation defoaming in 93~97 DEG C
After dip in glue, after 35~38 DEG C of dry 6~9h demoulding to get starch base hard capsule.
2. preparation method according to claim 1, which is characterized in that starch described in S1 be cornstarch, tapioca,
Potato starch any one or more of.
3. preparation method according to claim 1, which is characterized in that the reaction temperature of acidolysis described in S1 is 40 DEG C, instead
It is 12h between seasonable.
4. preparation method according to claim 1, which is characterized in that the volume fraction of propylene oxide described in S2 is 20%.
5. preparation method according to claim 1, which is characterized in that the reaction temperature being etherified described in S2 is 40 DEG C, instead
It is 22h between seasonable.
6. preparation method according to claim 1, which is characterized in that centrifugal rotational speed described in S1 and S2 is 5000r/min,
Centrifugation time is 10min.
7. preparation method according to claim 1, which is characterized in that starch described in S3 is each by following mass percent
Group is grouped as：Modified starch 40% and high amylose starches 60%.
8. preparation method according to claim 1, which is characterized in that the temperature of colloidal sol described in S3 is 95 DEG C.
9. preparation method according to claim 1, which is characterized in that dry temperature described in S3 is 35 DEG C, and the time is
6h。
10. the starch base hard capsule that any one of claim 1 to 9 the method is prepared is preparing drug, health products and work(
Application in energy food.
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| CN109452621A (en) * | 2018-11-01 | 2019-03-12 | 江南大学 | A kind of pH responsive type starch base microcapsules and preparation method thereof |
| CN109452621B (en) * | 2018-11-01 | 2022-04-15 | 江南大学 | pH-sensitive starch-based microcapsule and preparation method thereof |
| CN113121709A (en) * | 2019-12-30 | 2021-07-16 | 仙乐健康科技股份有限公司 | Preparation method and application of modified starch |
| CN112245589A (en) * | 2020-10-22 | 2021-01-22 | 甘肃世邦星达生物科技有限公司 | Modified starch for capsules and capsules |
| WO2022121370A1 (en) * | 2020-12-09 | 2022-06-16 | 江南大学 | Processing method for self-reinforced starch-based multifunctional material |
| CN112552555A (en) * | 2020-12-31 | 2021-03-26 | 河南省化工研究所有限责任公司 | Preparation method of modified high amylose-based plant capsule |
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