CN114044942B - Modified starch capsule shell and preparation method thereof - Google Patents
Modified starch capsule shell and preparation method thereof Download PDFInfo
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- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
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Abstract
The invention provides a preparation method of a modified starch capsule shell, which comprises the following steps: preparing starch slurry by adding water into amorphous granular treated starch, adding polydextrose, adjusting the starch slurry to be acidic, and performing ultrasonic treatment; s2, transferring the hydroxypropyl octyl succinic anhydride into the starch slurry obtained in the step S1, and pumping the starch slurry into a high-voltage pulse electric field treatment chamber at the temperature of 20-30 ℃ for modification treatment; s3, heating the modified starch slurry obtained in the step S2 to gelatinize, sequentially adding a plasticizer and a surfactant, and then carrying out constant temperature treatment at 80 ℃; and S4, cooling the starch glue solution obtained in the step S3, degassing in vacuum to remove bubbles, and then carrying out gluing, drying and demolding treatment to obtain a capsule shell. The capsule shell prepared by the invention not only has strong water resistance, is not easy to become brittle or soft under the influence of temperature and humidity, but also has good comprehensive performance in the aspects of disintegration time limit, viscosity, drying weight loss and the like.
Description
Technical Field
The invention relates to the technical field of modified starch, in particular to a modified starch capsule shell and a preparation method thereof.
Background
The traditional capsule shell is a gelatin product which is prepared by taking bones, skins and connective tissues of animals as raw materials and carrying out a series of complex physicochemical treatments, has high protein and no fat and is easy to be absorbed by human bodies. However, the capsule has the defects of volatile water hardening, water absorption softening, poor protection effect on moisture and oxygen sensitive medicines in the storage process, easy cross-linking reaction with aldehyde substances, delayed disintegration of the capsule shell, reduced medicine dissolution rate and the like. In addition, the development of the gelatin capsule industry encounters a series of difficulties and challenges due to the rapid rise of the price and frequent quality problems of gelatin, and the search for novel materials for preparing non-gelatin capsules becomes one of the development directions of current pharmaceutical excipients.
At present, novel non-gelatin soft capsule products represented by plant soft capsules such as cellulose derivatives, edible polysaccharide colloids and starch soft capsules and high polymer soft capsules are mainly formed in the research and development aspects of non-gelatin soft capsules. The modified starch is an inexhaustible natural product due to low price, and is a substitute of a most potential capsule shell raw material. However, due to the polyhydroxy structure of starch, the starch film has strong hydrophilicity and poor water resistance, and is easily affected by humidity, so that the capsule shell becomes brittle or soft, and strict storage conditions are required.
In order to solve the technical problem, researches are mostly carried out on preparing capsules by taking starch or modified starch as raw materials, a hydrophobing agent is usually adopted in the prior art to modify the starch or modified starch to prepare the capsules, but after the hydrophobing agent is modified, the toughness of the capsules cannot meet the requirement, so that a modified starch capsule shell which can improve the toughness and can prevent the capsules from being influenced by humidity is needed.
Disclosure of Invention
In view of the above, the invention provides a modified starch capsule shell which is not affected by humidity and maintains higher toughness, and a preparation method thereof.
The technical scheme of the invention is realized as follows: firstly, the invention provides a preparation method of a modified starch capsule shell, which comprises the following steps:
s1, treating starch in an amorphous granular state, adding water to prepare starch slurry with the mass fraction of 20-40%, adding polydextrose into the starch slurry, uniformly stirring, adjusting the pH value of the starch slurry to 5-7, and performing ultrasonic treatment for 2-3h;
s2, dissolving hydroxypropyl octyl succinic anhydride in an organic solvent, then transferring the solution into the starch slurry obtained in the step S1, adding 2mol/L of NaCl aqueous solution to adjust the conductivity of the starch slurry to 10-15mS/cm, and pumping the starch slurry into a high-voltage pulse electric field treatment chamber at the temperature of 20-30 ℃ for modification treatment;
s3, heating the modified starch slurry obtained in the step S2 to 70-90 ℃ for full gelatinization to obtain a starch glue solution, sequentially adding a plasticizer and a surfactant into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 0.5-1h to dissolve the starch glue solution into a uniform glue solution;
and S4, cooling the starch glue solution obtained in the step S3 to 40-50 ℃, performing vacuum degassing treatment for 0.5-1h to remove bubbles, and then performing gluing, drying and demolding treatment to obtain a capsule shell.
On the basis of the above technical solution, preferably, the amorphous particle state processing step in step S1 includes: mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1; after the reaction is finished, cooling to 20-30 ℃, washing for 3 times by using ethanol solution with volume fraction of 95%, carrying out vacuum filtration, drying, and sieving with a 120-mesh sieve to obtain amorphous granular starch.
On the basis of the above technical solution, preferably, the high voltage pulse processing parameters in step S2 are: the pulse amplitude is 18-20v, the pulse frequency is 800-1000Hz, the pulse width is 30-50 mus, and the pulse number is 150-180.
On the basis of the technical scheme, preferably, the polydextrose is polydextrose modified by a dynamic high-pressure microjet technology, and the modification method comprises the following steps: mixing polydextrose and distilled water according to the mass ratio of 1 (20-30), modifying for 3-5 times by adopting a high-pressure microjet technology homogenizer under the condition of 150-200Mpa, drying, crushing and sieving by a 200-mesh sieve to obtain the modified polydextrose.
On the basis of the technical scheme, preferably, the addition amount of the polydextrose is 3% -5% of the dry mass of the starch.
On the basis of the technical scheme, preferably, the addition amount of the hydroxypropyl octyl succinic anhydride is 0.5-3% of the dry mass of the starch.
On the basis of the technical scheme, preferably, the starch is one or a combination of more of corn starch, sweet potato starch and pea starch.
On the basis of the technical scheme, preferably, the plasticizer is one or a combination of more of hydroxypropyl methylcellulose, cellulose acetate, microcrystalline cellulose, glycerol and polyethylene glycol, and the addition amount of the plasticizer is 8-12% of the dry mass of the starch.
On the basis of the technical scheme, preferably, the surfactant is one or more of sodium dodecyl sulfate, glyceryl caprylate polyethylene glycol, sodium dioctyl sulfosuccinate, glycerol monooleate, polyvinyl alcohol and sorbitan laurate, and the addition amount of the surfactant is 1-5% of the dry mass of the starch.
On the basis of the above technical scheme, preferably, the organic solvent is ethanol or polyethylene glycol, and the hydroxypropyl octyl succinic anhydride: the mass ratio of the organic solvent is 1 (3-5).
Secondly, the invention provides a modified starch capsule shell which is prepared by the preparation method.
Compared with the prior art, the modified starch capsule shell and the preparation method thereof have the following beneficial effects:
(1) The polydextrose has the function of improving the tolerance of the capsule shell to the environment, and the dynamic high-pressure microjet technology enables the molecular mass of the polydextrose to be reduced and the particle size to be reduced, so that the polydextrose can better interact with long chains in starch, and the tolerance of the capsule shell to the temperature and humidity in the storage environment is improved.
(2) The invention adopts amorphous granular treated starch, improves the solubility and the reactivity of the starch and promotes the reaction of the starch and the polydextrose.
(3) The hydroxypropyl octyl succinic anhydride treated by the high-voltage pulse electric field modifies starch, can improve the water resistance of the starch, and has the functions of improving the temperature and humidity tolerance of a capsule shell and improving the disintegration time limit, friability, viscosity, drying weight loss and microbial limit to a certain extent by cooperating with polydextrose.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of a modified starch capsule shell comprises the following steps:
s1, mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1, adding corn starch to prepare starch slurry with a mass fraction of 30%, transferring the starch slurry into a closed reactor, heating to 85 ℃, and preserving heat for 30min under a 400Mpa environment; after the reaction is finished, cooling to 20 ℃, washing for 3 times by using an ethanol solution with the volume fraction of 95%, carrying out vacuum filtration, drying, and then sieving by using a 120-mesh sieve to obtain the amorphous granular starch.
And S2, adding water into the amorphous granular starch obtained in the step S1 to prepare starch slurry with the mass fraction of 20%, adding polydextrose into the starch slurry, uniformly stirring, adding citric acid to adjust the pH value of the starch slurry to 5, and performing ultrasonic treatment for 2 hours at the frequency of 20kHz, the power of 150W and the temperature of 20 ℃. The addition amount of polydextrose is 3 percent of the dry mass of starch.
S3, dissolving hydroxypropyl octyl succinic anhydride in polyethylene glycol, then transferring the solution into the starch slurry obtained in the step S2, adding 2mol/L NaCl aqueous solution to adjust the conductivity of the starch slurry to 10mS/cm, and pumping the starch slurry into a high-voltage pulse electric field treatment chamber at the temperature of 20 ℃ for modification treatment; the high-voltage pulse processing parameters are as follows: the pulse amplitude was 18v, the pulse frequency was 800Hz, the pulse width was 30. Mu.s, and the pulse number was 150. The addition amount of hydroxypropyl octyl succinic anhydride is 0.5 percent of the dry mass of the starch, and the weight ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of the polyethylene glycol is 1.
S4, heating the modified starch slurry obtained in the step S3 to 70 ℃ to be fully pasted into a starch glue solution, sequentially adding hydroxypropyl methylcellulose and sodium dodecyl sulfate into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 0.5-1h to dissolve the starch glue solution into a uniform glue solution; the addition amount of the hydroxypropyl methylcellulose is 8 percent of the dry mass of the starch, and the addition amount of the lauryl sodium sulfate is 1 percent of the dry mass of the starch.
And S5, cooling the starch glue solution obtained in the step S4 to 40 ℃, performing vacuum degassing treatment for 0.5h to remove bubbles, and then performing gluing, drying and demolding treatment to obtain the capsule shell.
Example 2
A preparation method of a modified starch capsule shell comprises the following steps:
s1, mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1; after the reaction is finished, cooling to 30 ℃, washing for 3 times by using an ethanol solution with the volume fraction of 95%, carrying out vacuum filtration, drying, and sieving by using a 120-mesh sieve to obtain the amorphous granular starch.
S2, mixing polydextrose and distilled water according to the mass ratio of 1.
And S3, adding water into the amorphous granular starch obtained in the step S1 to prepare starch slurry with the mass fraction of 40%, adding the modified polydextrose obtained in the step S2 into the starch slurry, uniformly stirring, adjusting the pH value of the starch slurry to 7, and performing ultrasonic treatment for 3 hours at the frequency of 50kHz, the power of 200W and the temperature of 50 ℃. The addition amount of polydextrose is 5 percent of the dry mass of starch.
S4, dissolving hydroxypropyl octyl succinic anhydride in ethanol, transferring the solution into the starch slurry obtained in the step S3, adding 2mol/L NaCl aqueous solution to adjust the conductivity of the starch slurry to be 15mS/cm, and pumping the starch slurry into a high-voltage pulse electric field processing chamber at 30 ℃ for modification treatment; the high-voltage pulse processing parameters are as follows: the pulse amplitude was 20v, the pulse frequency was 1000Hz, the pulse width was 50. Mu.s, and the pulse number was 180. The addition amount of hydroxypropyl octyl succinic anhydride is 3 percent of the dry mass of the starch. The hydroxypropyl octyl succinic anhydride: the mass ratio of ethanol is 1.
S5, heating the modified starch slurry obtained in the step S4 to 90 ℃ to be fully gelatinized into a starch glue solution, sequentially adding cellulose acetate and polyethylene glycol caprylic glyceride into the starch glue solution, and then carrying out constant-temperature treatment for 1 hour at the temperature of 80 ℃ to dissolve the starch glue solution into a uniform glue solution; the addition amount of the cellulose acetate is 12% of the dry mass of the starch, and the addition amount of the polyethylene glycol glyceryl caprylate is 5% of the dry mass of the starch.
And S6, cooling the starch glue solution obtained in the step S5 to 50 ℃, performing vacuum degassing treatment for 1 hour to remove bubbles, and then performing gluing, drying and demolding treatment to obtain a capsule shell.
Example 3
A preparation method of a modified starch capsule shell comprises the following steps:
s1, mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1; after the reaction is finished, cooling to 25 ℃, washing for 3 times by using an ethanol solution with the volume fraction of 95%, carrying out vacuum filtration, drying, and then sieving by using a 120-mesh sieve to obtain the amorphous granular starch.
S2, mixing polydextrose and distilled water according to the mass ratio of 1.
And S3, adding water into the amorphous granular starch obtained in the step S1 to prepare starch slurry with the mass fraction of 30%, adding the modified polydextrose obtained in the step S2 into the starch slurry, uniformly stirring, adding citric acid to adjust the pH value of the starch slurry to 6, and carrying out ultrasonic treatment for 2.5 hours under the conditions of the frequency of 30kHz, the power of 180W and the temperature of 30 ℃. The addition amount of the polydextrose is 4 percent of the dry base mass of the starch.
S4, dissolving hydroxypropyl octyl succinic anhydride in an organic solvent, then transferring the solution into the starch slurry obtained in the step S3, adding 2mol/L NaCl aqueous solution to adjust the conductivity of the starch slurry to be 12mS/cm, and pumping the starch slurry into a high-voltage pulse electric field processing chamber at 25 ℃ for modification treatment; the high-voltage pulse processing parameters are as follows: the pulse amplitude was 19v, the pulse frequency was 900Hz, the pulse width was 40. Mu.s, and the pulse number was 160. The addition amount of hydroxypropyl octyl succinic anhydride is 1 percent of the dry mass of the starch. The hydroxypropyl octyl succinic anhydride: the mass ratio of ethanol is 1.
S5, heating the modified starch milk obtained in the step S4 to 80 ℃ for full gelatinization to obtain a starch glue solution, sequentially adding microcrystalline cellulose and sodium dioctyl sulfosuccinate into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 40min to dissolve the starch glue solution into a uniform glue solution; the addition amount of the microcrystalline cellulose is 10% of the dry mass of the starch, and the addition amount of the dioctyl sodium sulfosuccinate is 2% of the dry mass of the starch.
And S6, cooling the starch glue solution obtained in the step S5 to 45 ℃, performing vacuum degassing treatment for 40min to remove bubbles, and then performing gluing, drying and demolding treatment to obtain the capsule shell.
Example 4
A preparation method of modified starch capsule shells comprises the following steps:
s1, mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1, adding corn starch to prepare starch slurry with a mass fraction of 45%, transferring the starch slurry into a closed reactor, heating to 85 ℃, and preserving heat for 30min under a 400Mpa environment; after the reaction is finished, cooling to 20 ℃, washing for 3 times by using an ethanol solution with the volume fraction of 95%, carrying out vacuum filtration, drying, and then sieving by using a 120-mesh sieve to obtain the amorphous granular starch.
S2, mixing polydextrose and distilled water according to the mass ratio of 1.
And S3, adding water into the amorphous granular starch obtained in the step S1 to prepare starch slurry with the mass fraction of 35%, adding the modified polydextrose obtained in the step S2 into the starch slurry, uniformly stirring, adjusting the pH of the starch slurry to 7, and performing ultrasonic treatment for 3 hours at the frequency of 40kHz, the power of 160W and the temperature of 40 ℃. The addition amount of the polydextrose is 4 percent of the dry basis weight of the corn starch.
S4, dissolving hydroxypropyl octyl succinic anhydride in polyethylene glycol, then transferring to the starch slurry obtained in the step S3, adding 2mol/L NaCl aqueous solution to adjust the conductivity of the starch slurry to 10mS/cm, and pumping the starch slurry into a high-voltage pulse electric field processing chamber at the temperature of 20 ℃ for modification treatment; the high-voltage pulse processing parameters are as follows: the pulse amplitude was 18v, the pulse frequency was 800Hz, the pulse width was 30. Mu.s, and the pulse number was 150. The addition amount of hydroxypropyl octyl succinic anhydride is 2 percent of the dry mass of the starch, and the ratio of hydroxypropyl octyl succinic anhydride: the mass ratio of the polyethylene glycol is 1.
S5, heating the modified starch milk obtained in the step S4 to 75 ℃ to be fully pasted into a starch glue solution, sequentially adding glycerol and glycerol monooleate into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 0.5h to dissolve the starch glue solution into a uniform glue solution; the addition amount of the glycerol is 11% of the dry mass of the starch, and the addition amount of the glycerol monooleate is 4% of the dry mass of the starch.
And S6, cooling the starch glue solution obtained in the step S5 to 50 ℃, performing vacuum degassing treatment for 1 hour to remove bubbles, and then performing gluing, drying and demolding treatment to obtain a capsule shell.
Example 5
A preparation method of a modified starch capsule shell comprises the following steps:
s1, mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1; after the reaction is finished, cooling to 25 ℃, washing for 3 times by using an ethanol solution with the volume fraction of 95%, carrying out vacuum filtration, drying, and sieving by using a 120-mesh sieve to obtain the amorphous granular starch. Corn starch: the pea starch mass ratio is 2.
S2, mixing polydextrose and distilled water according to the mass ratio of 1.
And S3, adding water into the amorphous granular starch obtained in the step S1 to prepare starch slurry with the mass fraction of 25%, adding the modified polydextrose obtained in the step S2 into the starch slurry, uniformly stirring, adding citric acid to adjust the pH value of the starch slurry to 5, and carrying out ultrasonic treatment for 3 hours under the conditions of frequency of 40kHz, power of 160W and temperature of 40 ℃. The addition amount of the polydextrose is 5 percent of the dry base mass of the starch.
S4, dissolving hydroxypropyl octyl succinic anhydride in an organic solvent, then transferring the solution into the starch slurry obtained in the step S3, adding 2mol/L NaCl aqueous solution to adjust the conductivity of the starch slurry to 11mS/cm, and pumping the starch slurry into a high-voltage pulse electric field treatment chamber at 28 ℃ for modification treatment; the high-voltage pulse processing parameters are as follows: the pulse amplitude was 20v, the pulse frequency was 850Hz, the pulse width was 45. Mu.s, and the pulse number was 170. The addition amount of hydroxypropyl octyl succinic anhydride is 2.5 percent of the dry mass of the starch, and the weight ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of ethanol is 1.
S5, heating the modified starch milk obtained in the step S4 to 85 ℃ for full gelatinization to obtain a starch glue solution, sequentially adding cellulose acetate, microcrystalline cellulose, polyvinyl alcohol and sorbitan laurate into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 1h to dissolve the starch glue solution into a uniform glue solution; the addition amount of the cellulose acetate and the microcrystalline cellulose is respectively 4% and 5% of the dry basis mass of the starch; the addition amount of the polyvinyl alcohol and the sorbitan laurate is 2 percent and 3 percent of the dry mass of the starch.
And S6, cooling the starch glue solution obtained in the step S5 to 40 ℃, performing vacuum degassing treatment for 0.5 hour to remove bubbles, and then performing gluing, drying and demolding treatment to obtain a capsule shell.
Comparative example 1
The method is characterized in that ordinary corn starch which is not processed in an amorphous granular state is used as a starch raw material, an example 1 without adding polydextrose is used as a comparative example 1, and the rest of the reagents and steps are the same as those in the example 1, and the method specifically comprises the following steps:
a preparation method of modified starch capsule shells comprises the following steps:
s1, adding water into corn starch to prepare starch slurry with the mass fraction of 20%, and carrying out ultrasonic treatment for 2 hours under the conditions of frequency of 20kHz, power of 150W and temperature of 20 ℃.
And S2, dissolving hydroxypropyl octyl succinic anhydride in polyethylene glycol, transferring the solution into the starch slurry obtained in the step S1, and stirring and reacting for 2 hours at the temperature of 40 ℃ to obtain the modified starch milk. The addition amount of hydroxypropyl octyl succinic anhydride is 0.5 percent of the dry mass of the starch, and the ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of the polyethylene glycol is 1.
S3, dissolving hydroxypropyl octyl succinic anhydride in polyethylene glycol, then transferring to the starch slurry obtained in the step S2, adding 2mol/L NaCl aqueous solution to adjust the conductivity of the starch slurry to 10mS/cm, and pumping the starch slurry into a high-voltage pulse electric field processing chamber at the temperature of 20 ℃ for modification treatment; the high-voltage pulse processing parameters are as follows: the pulse amplitude was 18v, the pulse frequency was 800Hz, the pulse width was 30. Mu.s, and the pulse number was 150. The addition amount of hydroxypropyl octyl succinic anhydride is 0.5 percent of the dry mass of the starch, and the ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of the polyethylene glycol is 1.
S4, heating the modified starch slurry obtained in the step S3 to 70 ℃ to be fully pasted into a starch glue solution, sequentially adding hydroxypropyl methylcellulose and sodium dodecyl sulfate into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 0.5-1h to dissolve the starch glue solution into a uniform glue solution; the addition amount of the hydroxypropyl methylcellulose is 8 percent of the dry mass of the starch, and the addition amount of the lauryl sodium sulfate is 1 percent of the dry mass of the starch.
And S5, cooling the starch glue solution obtained in the step S4 to 40 ℃, performing vacuum degassing treatment for 0.5h to remove bubbles, and then performing gluing, drying and demolding treatment to obtain the capsule shell.
Comparative example 2
Common corn starch is used as a starch raw material, glucan is added, hydroxypropyl octyl succinic anhydride is used for modifying the starch under the alkaline condition, and other reagents and steps are the same as those in the example 1, and the details are as follows:
a preparation method of modified starch capsule shells comprises the following steps:
s1, adding water into corn starch to prepare starch slurry with the mass fraction of 20%, adding polydextrose into the starch slurry, uniformly stirring, adjusting the pH value of the starch slurry to 5, and performing ultrasonic treatment for 2 hours at the frequency of 20kHz, the power of 150W and the temperature of 20 ℃. The addition amount of the polydextrose is 3 percent of the dry base mass of the starch.
S2, dissolving hydroxypropyl octyl succinic anhydride in polyethylene glycol, transferring to the starch slurry obtained in the step S1, adding NaOH to adjust the pH value of the starch slurry to 8, and stirring and reacting for 2 hours at the temperature of 40 ℃ to obtain the modified starch milk. The addition amount of hydroxypropyl octyl succinic anhydride is 0.5 percent of the dry mass of the starch, and the ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of the polyethylene glycol is 1.
S3, heating the modified starch milk obtained in the step S2 to 70 ℃ to be fully pasted into a starch glue solution, sequentially adding hydroxypropyl methylcellulose and lauryl sodium sulfate into the starch glue solution, and then carrying out constant-temperature treatment for 0.5-1h at the temperature of 80 ℃ to dissolve the starch glue solution into a uniform glue solution; the addition amount of the hydroxypropyl methylcellulose is 8 percent of the dry mass of the starch, and the addition amount of the lauryl sodium sulfate is 1 percent of the dry mass of the starch.
And S4, cooling the starch glue solution obtained in the step S3 to 40 ℃, performing vacuum degassing treatment for 0.5h to remove bubbles, and then performing gluing, drying and demolding treatment to obtain the capsule shell.
Comparative example 3
The method is the same as example 1 in the steps of taking common corn starch which is not processed in an amorphous granular state as a starch raw material, adding no polydextrose, and modifying the starch by using hydroxypropyl octyl succinic anhydride under an alkaline condition, wherein the steps of the other reagents are as follows:
a preparation method of a modified starch capsule shell comprises the following steps:
s1, adding water into corn starch to prepare starch slurry with the mass percent of 20%, and carrying out ultrasonic treatment for 2 hours under the conditions of frequency of 20kHz, power of 150W and temperature of 20 ℃.
And S2, dissolving hydroxypropyl octyl succinic anhydride in polyethylene glycol, transferring to the starch slurry obtained in the step S1, adding NaOH to adjust the pH value of the starch slurry to 8, and stirring and reacting for 2 hours at the temperature of 40 ℃ to obtain the modified starch milk. The addition amount of hydroxypropyl octyl succinic anhydride is 0.5 percent of the dry mass of the starch, and the ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of the polyethylene glycol is 1.
S3, heating the modified starch milk obtained in the step S2 to 70 ℃ to be fully pasted into a starch glue solution, sequentially adding hydroxypropyl methylcellulose and sodium dodecyl sulfate into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 0.5-1h to dissolve the starch glue solution into a uniform glue solution; the addition amount of the hydroxypropyl methylcellulose is 8 percent of the dry mass of the starch, and the addition amount of the lauryl sodium sulfate is 1 percent of the dry mass of the starch.
And S4, cooling the starch glue solution obtained in the step S3 to 40 ℃, performing vacuum degassing treatment for 0.5 hour to remove bubbles, and then performing gluing, drying and demolding treatment to obtain a capsule shell.
And (3) testing the temperature and humidity tolerance of the capsule shell: placing the capsule shell at high temperature and high humidity: temperature 50 ℃, humidity 80% environment 24h: low temperature and low humidity: the temperature is 5 ℃, and the humidity is 30% for 24 hours; the degree of soft deformation or friability of the capsule shell is observed, the friability is detected by referring to the item of gelatin hollow capsules in 2010 edition of pharmacopoeia of the people's republic of China, 50 capsules are detected in each example or comparative example, and the detection results are shown in table 1.
TABLE 1 test result table of temperature and humidity tolerance of capsule shell
The data in table 1 show that the temperature and humidity resistance of the capsule shell is example > comparative example 2> comparative example 1> comparative example 3, which shows that the dynamic high-pressure microjet technology reduces the molecular mass of the polydextrose, reduces the particle size, and enables the polydextrose to better interact with long chains in starch, thereby improving the temperature and humidity resistance of the capsule shell in the storage environment. The solubility and the reactivity of the starch processed in the amorphous granular state are improved, the reaction of the starch and the polydextrose is promoted, and the tolerance of the capsule shell to temperature and humidity is favorably improved. The capsule shell prepared by the invention has no obvious change no matter the capsule shell is placed in the environment with low temperature and low humidity or high temperature and high humidity, keeps good characteristics and does not need harsh storage conditions.
Quality index of capsule shell: the detection of the tightness, the disintegration time limit, the friability, the viscosity, the drying weight loss and the microbial limit refers to the detection of gelatin empty capsules item in the 2010 version of pharmacopoeia of the people's republic of China, 50 capsules are detected in each embodiment or comparative example, and the detection results are shown in table 2.
TABLE 2 Capsule Shell quality index test result table
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Degree of tightness | Without leaking powder | Without leaking powder | Without leaking powder | Without powder leakage | Without leaking powder | Without leaking powder | Without leaking powder | Powder leakage |
| Disintegration time limit (min) | <1 | <1 | <1 | <1 | <1 | 6 | 8 | 10 |
| Friability (grain) | 2 | 0 | 1 | 0 | 1 | 8 | 6 | 13 |
| Viscosity (mm) 2 /s) | 81 | 83 | 85 | 83 | 85 | 60 | 53 | 47 |
| Loss on drying (%) | 8.25 | 8.17 | 8.05 | 7.36 | 6.89 | 10.9 | 12.5 | 14.8 |
| Limit of microorganism | Qualified | Qualified | Qualified | Qualified | Qualified | Qualified | Fail to be qualified | Fail to be qualified |
The data in Table 2 show that the capsule shell of the invention has high adhesion, short disintegration time, lower drying weight loss, qualified microbial limit and good comprehensive performance. The hydroxypropyl octyl succinic anhydride treated by the high-voltage pulse electric field modifies starch, can improve the water resistance of the starch, and has the functions of improving the temperature and humidity tolerance of a capsule shell and improving the disintegration time limit, friability, viscosity, drying weight loss and microbial limit to a certain extent by cooperating with polydextrose.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (6)
1. A preparation method of a modified starch capsule shell is characterized by comprising the following steps:
s1, treating starch in an amorphous granular state, adding water to prepare starch slurry with the mass fraction of 20-40%, adding polydextrose into the starch slurry, uniformly stirring, adjusting the pH value of the starch slurry to 5-7, and performing ultrasonic treatment for 2-3h; the addition amount of the polydextrose is 3-5% of the dry mass of the starch;
s2, dissolving hydroxypropyl octyl succinic anhydride in an organic solvent, then transferring the solution into the starch slurry subjected to ultrasonic treatment in the step S1, adding 2mol/L of NaCl aqueous solution to adjust the conductivity of the starch slurry to 10-15mS/cm, and pumping the starch slurry into a high-voltage pulse electric field treatment chamber at the temperature of 20-30 ℃ for modification treatment; the organic solvent is ethanol or polyethylene glycol, the addition amount of the hydroxypropyl octyl succinic anhydride is 0.5-3% of the dry mass of the starch, and the weight ratio of the hydroxypropyl octyl succinic anhydride: the mass ratio of the organic solvent is 1 (3-5); the high-voltage pulse processing parameters are as follows: the pulse amplitude is 18-20v, the pulse frequency is 800-1000Hz, the pulse width is 30-50 mus, and the pulse number is 150-180;
s3, heating the modified starch slurry obtained in the step S2 to 70-90 ℃ for full gelatinization to obtain a starch glue solution, sequentially adding a plasticizer and a surfactant into the starch glue solution, and then carrying out constant-temperature treatment at 80 ℃ for 0.5-1h to dissolve the starch glue solution into a uniform glue solution;
s4, cooling the starch glue solution obtained in the step S3 to 40-50 ℃, performing vacuum degassing treatment for 0.5-1h to remove bubbles, and then performing gluing, drying and demolding treatment to obtain a capsule shell;
step S1, the amorphous grain state processing step comprises: mixing absolute ethyl alcohol and distilled water according to a volume ratio of 1; after the reaction is finished, cooling to 20-30 ℃, washing for 3 times by using ethanol solution with volume fraction of 95%, carrying out vacuum filtration, drying, and then sieving by using a 120-mesh sieve to obtain amorphous granular starch.
2. A process for the preparation of a modified starch capsule shell as claimed in claim 1, wherein: the polydextrose is modified by a dynamic high-pressure microjet technology, and the modification method comprises the following steps: mixing polydextrose and distilled water according to the mass ratio of 1 (20-30), modifying for 3-5 times by adopting a high-pressure microjet technology homogenizer under the condition of 150-200Mpa, drying, crushing and sieving by a 200-mesh sieve to obtain the modified polydextrose.
3. The process for preparing a modified starch capsule shell according to claim 1, wherein: the starch is one or more of corn starch, sweet potato starch and pea starch.
4. The process for preparing a modified starch capsule shell according to claim 1, wherein: the plasticizer is one or a combination of more of hydroxypropyl methylcellulose, cellulose acetate, microcrystalline cellulose, glycerol and polyethylene glycol, and the addition amount of the plasticizer is 8-12% of the dry basis weight of the starch.
5. The process for preparing a modified starch capsule shell according to claim 1, wherein: the surfactant is one or a combination of more of sodium dodecyl sulfate, polyethylene glycol glyceryl caprylate, dioctyl sodium sulfosuccinate, glycerol monooleate, polyvinyl alcohol and sorbitan laurate, and the addition amount of the surfactant is 1-5% of the dry mass of the starch.
6. A modified starch capsule shell prepared by the method for preparing a modified starch capsule shell according to any one of claims 1 to 5.
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