CN105832696A

CN105832696A - Preparation method of starch hollow capsule

Info

Publication number: CN105832696A
Application number: CN201610189157.2A
Authority: CN
Inventors: 郭帅达
Original assignee: Individual
Current assignee: Individual
Priority date: 2016-03-24
Filing date: 2016-03-24
Publication date: 2016-08-10

Abstract

The invention relates to a preparation method of a starch hollow capsule. The preparation method comprises preparing a dispersion liquid with a concentration of 20-40% from 60-80 parts of modified starch, 10-20 parts of a plasticizer and 1-5 parts of a thickening agent, completely gelatinating and dissolving starch at a temperature of 80 DEG C, carrying out cooling to a temperature of 50 DEG C, carrying out gel dipping molding through a capsule mold 1#, carrying out drying at a temperature of 38 DEG C for 1h and carrying out demolding, cutting and sleeving to obtain the starch hollow capsule. The plasticizer is isosorbide. After isosorbide contacts with a starch macromolecule, isosorbide does not easily go out of a starch system through a rigid annular structure so that good mechanical properties of the starch hollow capsule are kept for a long time. The starch hollow capsule has a cost half of a gelatin capsule cost and has generalizability and applicability.

Description

A kind of preparation method of starch hollow capsule

Technical field

The invention belongs to field of medicine preparation, relate to a kind of starch hollow capsule preparation method.

Background technology

Medicinal hollow capsule is the bladder that extraordinary filmogen is made, while the protection medicine property of medicine is not destroyed, to human body Digestive organs and respiratory tract also have good protective effect.Compared with tablet, the watered pill, capsule has drug bioavailability The advantages such as high, raising medicine stability, have been obtained for being widely applied in pharmaceutical preparation industry.The softgel shell of conventional capsules is main Being made up of gelatin, the physicochemical property of animal sources gelatin itself and the complexity in source, resistance to control determine product and there is many being difficult to The performance overcome and the defect of secure context.As above latter stage in century, the state such as American-European broken out large-area " bovine spongiform encephalopathy ", Yi Jiwo At the beginning of state 2012, " the toxic capsule event " of outburst allows the drawback of tradition gelatine capsule show fully especially.Therefore, exploitation non-animal Plant capsule shell material replace gelatin to receive the extensive concern of people.

From the standpoint of the popularity in the prices of raw materials and source, starch is considered as most potential capsule raw material, if will form sediment Powder, as capsule shells wall material, can make up the defect of plant capsule expensive raw material price and gelatine capsule.But there is film property in starch The shortcomings such as difference, toughness are bad, accordingly, it would be desirable to be modified processing to starch according to the physicochemical property of starch, so that starch tool There is more excellent character, meet the requirement of reality application.

Summary of the invention

It is an object of the invention to provide a kind of starch hollow capsule preparation method.

By starch is carried out chemical modification, improve the strong hydrophilicity performance of starch material；By different plasticizers is contrasted, Preferably isosorbide is plasticizer, improves the fragility of starch-based material and can effectively suppress migration of plasticizer, it is thus achieved that mechanical property Excellent starch hollow capsule.Starch hollow capsule preparation method is:

Modified starch 60-80 part, plasticizer 10-20 part and 1-5 part thickening agent are made the dispersion liquid of concentration 20-40%, at 80 DEG C The complete gelatinizing of starch is dissolved, and is then cooled to 50 DEG C, utilizes capsule 1# mould to dip in gum forming, drying 1h at 38 DEG C, the demoulding, Starch hollow capsule is i.e. prepared after cutting, fit.The starch that the present invention mentions can be etherificate, esterification or Oxytarch； Plasticizer is isosorbide, and thickening agent can be agar, Pullulan glue or carrageenan etc..

Because capsule shells is ellipsoid shape, it is difficult to directly measuring its mechanical property, our employing is prepared composite starch film mode and investigated its power Learning performance, the preparation of composite starch film uses the tape casting, by 70-80 part substitution value be 0.6 starch acetate and plasticizer ethylene glycol, Glycerol, sorbitol or isosorbide 20-40 part add in cold water after dispersion, and being configured to mass concentration is 5%wt emulsion, is heated to 80 DEG C To the complete gelatinizing of starch, pour in frosting ware, in baking oven, at 50 DEG C, dry 5～7h, i.e. prepare composite starch film, multiple The mechanical property closing film is shown in Table 1.Starch hollow capsule prepared by the present invention and gelatine capsule performance comparison are shown in Table 2

Beneficial effect

From the point of view of the initial mechanical performance of material, four kinds of plasticizers all show the plasticising performance good to starch acetate.And After placing one month, use the starch composite membrane mechanical property of glycerol, ethylene glycol and sorbitol plasticising in the trend that significantly becomes fragile. This is likely due to what two kinds of reasons caused, and on the one hand starch film is in storage, produces because of constantly associating of molecule interchain hydrogen bond Raw aging, cause starch film to become fragile；On the other hand, plasticizer in composite film material not with starch polymer chemical bonding, They can move freely in macromolecular material, is prone to move to surface from material matrix, thus result in storage Film material flexibility declines.It should be noted that and use its hot strength of composite membrane of isosorbide plasticising and elongation at break through 1 After the storage of individual month, amplitude of variation is less, and the molecular structure that this may be special with isosorbide is relevant.Isosorbide molecule is by two Furan condensed ring forms, and its two five-ring heterocycles are V-shaped, and containing two hydroxyls, molecular structure has the biggest rigidity.When different mountain After pears alcohol contacts with starch polymer, the circulus of rigidity makes it be difficult to from starch system to move out, and then it is good to maintain material Good mechanical property (being shown in Table 1).

The starch hollow capsule cost of the present invention is greatly reduced with gelatine capsule ratio, and cost falls below the half of gelatine capsule, has Can application.

Accompanying drawing explanation

(A. corn starch, B. substitution value is the shallow lake of 0.6 to the infrared spectrogram of Fig. 1 corn starch and DS 0.6 starch acetate Powder acetate).

Fig. 2 starch hollow capsule photo

Detailed description of the invention

Embodiment 1, starch and glacial acetic acid are joined the 250mL there-necked flask being furnished with reflux condensing tube, agitating device and thermometer In, the mass concentration of starch is 32%；80 DEG C of temperature it are warming up to after mix and blend 5min；Adding with starch quality ratio is 1: 1 Acetic anhydride reaction 15min, add starch weight 1% Loprazolam, reaction 10min after filtration under diminished pressure, wash away with distilled water Debris is dried to constant weight and is i.e. prepared starch acetate；By starch acetate: isosorbide: carrageenan, three's mass ratio is 78: 20: 2, disperse in cold water, dispersion liquid concentration is 25%, dissolves 80 DEG C of complete gelatinizings of starch, is then cooled to 50 DEG C, Utilize capsule 1# mould to dip in gum forming, dry 1h at 45 DEG C, after the demoulding, cutting, fit, i.e. prepare starch hollow capsule.

After the present invention is reacted by starch esterification, the part of hydroxyl of starch by acetyl group replace (see Fig. 1), reduce with water it Between interaction improve starch hydrophilic.Sample infrared analysis test BRUKER Vertex 70FTIR (Madison, Germany) carrying out on type infrared spectrum analyser, resolution is 4cm^-1, sweep limits is 4000-400cm^-1, KBr tabletting, sample Being 5/200mg with KBr ratio, do background scans with KBr, before test, sample, under the conditions of 50 DEG C, is dried to constant weight.? Utilizing acetic anhydride and acetic acidreaction to be prepared for starch acetate in glacial acetic acid medium, the infrared structure of sample is as shown in Figure 1.With former The spectrogram of starch is compared, on the infrared spectrum of starch acetate, at 1754cm^-1、1435cm^-1、1375cm^-1、1240cm^-1 Near occur in that new absworption peak, be ester C=O stretching vibration peak, the asymmetric and symmetrical deformation vibration of CH3 and ester C respectively -O stretching vibration peak.At 1032cm^-1The new absworption peak that place occurs, is owing to the acetyl group of esterification introducing is to sugar ring vibration Impact, cause sugar ring symmetric vibration move to high wave number.Above data confirm to there occurs esterification, successfully synthesize Starch acetate.

The substitution value of starch acetate uses the method for nuclear-magnetism to calculate, and by regulating the consumption of acetic anhydride, is prepared for substitution value respectively It it is the starch acetate of 0.2,0.4 and 0.6.The introducing of acetate group in starch polymer structure, will make the parent of starch-based material Aqueous can obtain a certain degree of improvement.The hydrophobic performance of different degree of substitution starch acetate has been investigated, knot by contact angle experiments Fruit is as shown in table 1.Ative starch shows relatively low contact angle, because ative starch is polyol, and the affinity of water is relatively By force, after distilled water is added drop-wise to starch surface, water droplet be can be observed and quickly sprawl on its surface and come.After esterification, portion Divide hydroxyl to be replaced by acetyl group, reduce the interaction between water, so when the increase of substitution value, starch acetate Contact angle increase therewith.Contact angle test confirms that the introducing of acetate groups improves its hydrophilic and hydrophobic to a certain extent Energy.

Embodiment 2, by Oxytarch: isosorbide: Pullulan glue, three's mass ratio is 63: 35: 2, in cold water disperse, Dispersion liquid concentration is 35%, dissolves 80 DEG C of complete gelatinizings of starch, is then cooled to 50 DEG C, utilizes capsule 1# mould to dip in gum forming, Dry 1h at 38 DEG C, after the demoulding, cutting, fit, i.e. prepare starch hollow capsule.

The different plasticizer kind of table 1 and consumption are on composite membrane hot strength and the impact of elongation at break.

Table 2 starch hollow capsule all technical contrasts with gelatine capsule.

	Gelatine capsule	Starch capsule
			Gelatin viscosity	＜ 1500CP	20～30cp
Forming temperature	＜ 65 DEG C	50℃
			Dry temperature	＜ 50 DEG C	38℃
Drying time	＜ 3h	1h20min
			Disintegration time	＜ 10min	7～8min
Water content	13～18%	10～15%
			Cost of material is estimated	0.7 point/	0.4 point/

Table 3 ative starch and the contact angle of different degree of substitution starch acetate.

Claims

1. a starch hollow capsule preparation method, makes modified starch 60-80 part, plasticizer 10-20 part and 1-5 part thickening agent The dispersion liquid of concentration 20-40%, dissolves 80 DEG C of complete gelatinizings of starch, is then cooled to 50 DEG C, utilizes capsule 1# mould to dip in glue Molding, dries 1h, i.e. prepares starch hollow capsule, it is characterised in that described plasticizer after the demoulding, cutting, fit at 38 DEG C For isosorbide.

2. a kind of starch hollow capsule preparation method as claimed in claim 1, modified starch is starch acetate, and its manufacture method is Starch and glacial acetic acid join in the 250mL there-necked flask being furnished with reflux condensing tube, agitating device and thermometer, and the quality of starch is dense Degree is 32%；80 DEG C of temperature it are warming up to after mix and blend 5min；Add and react 15min with the acetic anhydride that starch quality ratio is 1: 1, Add the Loprazolam of starch weight 1%, filtration under diminished pressure after reaction 10min, wash away debris drying with distilled water and i.e. make to constant weight Obtain starch acetate.