CN103243140B - Preparation method of composite cyclodextrin - Google Patents

Abstract

The invention discloses a preparation method of composite cyclodextrin and belongs to the technical field of cyclodextrin. According to the method, corn starch is used as a substrate, and cyclodextrin glycosyl transferase (CGTase) of the Amano enzyme manufacturing (China), Ltd. is used to catalyze starch to prepare the composite cyclodextrin. The composite cyclodextrin related to the invention contains alpha-, beta-and gamma-cyclodextrin mixtures and malto-oligosaccharide, and the ratio of the four ingredients can be correspondingly varied according to the adjustment of a preparation technology. The preparation method has the advantages that the utilization efficiency of the starch substrate can be improved by about 90%; the solubility of single cyclodextrin can be improved; and the solid content can be increased, and the production cost is lowered.

Description

A kind of preparation method of complex loop dextrin

Technical field

A preparation method for complex loop dextrin, belongs to cyclodextrin technical field.

Background technology

Since last century the nineties, starch industry is progressively grown into national strategy industry, is successively listed in country " 15 ", Eleventh Five-Year Plan emphasis support items.During " 12 ", the major fields of β-amylose industry and study of investment opportunities thereof become hot issue.And W-Gum is topmost kind in starch, account for 80% of world's starch total amount.Carry out the comprehensive utilizating research of W-Gum to complying with " 12 " demand for development, realize Grain Development and efficiently rise in value, significant.

Cyclodextrin is as an important branch of β-amylose; there is the performances such as good chemical stability, thermostability, resistance to enzymolysis, moisture resistance because of it; can with scope extremely widely all kinds of objects form host-guest inclusion thing by molecular interaction; thereby object is had shielding, controls the functions such as release, active protection; be widely applied to the industry fields such as food, medicine, makeup, agricultural chemicals, material, penetrated into each corner of our life.It should with country for policy and the market environment of the high-valued processing of starch, there is the huge market requirement, be star's product that a tool has great prospects for development.

The present invention is taking cheap W-Gum as starting point, to improve the utilization ratio of starch and the service efficiency of improving cyclodextrin as target, by preparation process condition is explored, prepare and both contain α, beta, gamma-cyclodextrin contains again the complex loop dextrin product of oligose.Compared with traditional cyclodextrin preparation technology, the present invention can be according to the ratio that need to adjust α, β, tri-kinds of cyclodextrin of γ of application, process controllability is strong, be small molecular sugar by the unconverted starch degradation for cyclodextrin, the utilising efficiency that both can greatly improve starch, can increase again product solid content, has also improved the effect of cyclodextrin, be conducive to expand the embedding field of cyclodextrin, reduce the cost of embedding product.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of complex loop dextrin.

Technical scheme of the present invention: a kind of preparation method of complex loop dextrin, taking W-Gum as raw material, through degreasing, gelatinization, employing amano enzyme preparation Maltose 4-glucosyltransferase (CGTase) catalysis W-Gum, again through adding beta-amylase, Pullulanase and saccharifying enzyme conversion, activated carbon decolorizing, vacuum-drying etc., prepare and contain α, beta, gamma-cyclodextrin contains again the complex loop dextrin of oligose.Determine the operational path of CGTase catalysis W-Gum reaction, the consumption of starch substrates in the Catalytic processes of CGTase, the addition of CGTase zymin and reaction times.

Step is:

(1) starch degreasing

Take appropriate W-Gum, the quality methyl alcohol such as use to infiltrate, at 80 DEG C, boil 5min, filter, repeatable operation 3 times, thus carry out degreasing;

Degreasing object: the fat abstraction of W-Gum can reduce starting temperature, peak temperature, the final temperature of starch, also can make gelatinization scope increase simultaneously;

(2) starch pasting

Take W-Gum 100g after degreasing and be placed in the beaker of 400mL, add the water of 200mL, stir, in 62-72 DEG C of water-bath, heat, and continuous stir about 1h, starch slurry by starting gelatinization until completely become to stick with paste;

(3) add CGTase enzyme and add CGTase enzyme

Add CGTase enzyme liquid 400 U/g starch, at 75 DEG C, react 1 h, be cooled to 55 DEG C of the optimal reactive temperatures of enzyme; Again add CGTase enzyme liquid 400 U/g starch, 55 DEG C of reaction 20 h; In boiling water bath, heat 20 min termination reactions; Taking the reaction solution that do not add CGTase enzyme as blank, all the other operations are identical;

(4) adding beta-amylase, Pullulanase and saccharifying enzyme transforms

In step (3) gained reaction solution, add beta-amylase 100 U/g starch, Pullulanase 200 U/g starch and saccharifying enzyme 100 U/g starch, 50 DEG C of reaction 5 h, then boiling water bath heats 20 min termination reactions, makes the starch of unreacted be converted into small molecular sugar;

(5) activated carbon decolorizing

To the granulated active carbon that adds quality product 3% in step (4) products obtained therefrom, 80 DEG C of heating 30 min, filter the sample mix solution obtaining for three times through decolouring repeatedly;

(6) vacuum-drying

By step (5) gained through decolouring sample mix solution vacuumize dry, control drying temperature be 60 DEG C, be 8h time of drying, must contain α-, β-, γ-cyclodextrin contains again the complex loop dextrin product of oligose.

Beneficial effect of the present invention: complex loop dextrin involved in the present invention comprise α-, β-, γ-cyclodextrin mixture and malto-oligosaccharide, can there is corresponding variation with preparation technology's adjustment in the ratio of four kinds of compositions.The invention has the advantages that (1) can make the utilising efficiency of starch substrates bring up to approximately 90%.(2) can improve the solubleness of single cyclodextrin.(3) can increase solid content, reduce production costs.

Brief description of the drawings

Fig. 1 complex loop dextrin product preparation process FB(flow block).

The impact of Fig. 2 substrate addition on compound beta-cyclodextrin yield.

Embodiment

Embodiment 1

The impact of concentration of substrate on complex loop dextrin product

Adjust concentration of substrate and be respectively 2.5%, 5%, 10%, 15%, adding CGTase enzyme amount is 400 U/g starch, and reaction conditions is pH7.0,75 DEG C of first stage temperature; Subordinate phase adds CGTase enzyme amount 400U/g, 55 DEG C of temperature of reaction, other techniques are with reference to above-mentioned cyclodextrin preparation process, find the increase along with starch substrates concentration in reaction system, cyclodextrin transformation efficiency also declines gradually, and the transformation efficiency ratio of three kinds of cyclodextrin (see figure 2) has also occurred to change shows that the ratio of preparing cyclodextrin mixt in complex loop dextrin can adjust along with reaction conditions.

Embodiment 2

Complex loop dextrin product quality

When 25 DEG C of room temperatures, the solubleness of this product reaches 10.3g/100mL water, has improved more than 5 times than beta-cyclodextrin solubleness (1.88g/100mL water).So have higher water-soluble than single beta-cyclodextrin product.Application prospect is more more wide than beta-cyclodextrin.General weak acid can not be hydrolyzed complex loop dextrin product as acetic acid, and therefore the chemical property of this product is very stable; This product is at 100 DEG C of heating 30min, and weight is substantially without considerable change, good thermal stability; This product, in the time that RH is 84%, occurs without moisture absorption phenomenon substantially.

Claims (1)

1. the preparation method of a complex loop dextrin, it is characterized in that: taking W-Gum as raw material, through degreasing, gelatinization, employing Maltose 4-glucosyltransferase CGTase catalysis W-Gum, again through adding beta-amylase, Pullulanase and saccharifying enzyme conversion, activated carbon decolorizing, vacuum-drying, prepare and contain α, beta, gamma-cyclodextrin contains again the complex loop dextrin of oligose; Step is:

(1) degreasing

Take appropriate W-Gum, the quality methyl alcohol such as use to infiltrate, at 80 DEG C, boil 5min, filter, repeatable operation 3 times, thus carry out degreasing;

(2) gelatinization

Take W-Gum 100g after degreasing and be placed in the beaker of 400mL, add the water of 200mL, stir, in 62-72 DEG C of water-bath, heat, and constantly stir 1h, starch slurry by starting gelatinization until completely become to stick with paste;

(3) add CGTase enzyme and add CGTase enzyme

Add CGTase enzyme liquid 400 U/g starch, at 75 DEG C, react 1 h, be cooled to 55 DEG C of the optimal reactive temperatures of enzyme; Again add CGTase enzyme liquid 400 U/g starch, 55 DEG C of reaction 20 h; In boiling water bath, heat 20 min termination reactions; Taking the reaction solution that do not add CGTase enzyme as blank, all the other operations are identical;

(4) adding beta-amylase, Pullulanase and saccharifying enzyme transforms

In step (3) gained reaction solution, add beta-amylase 100 U/g starch, Pullulanase 200 U/g starch and saccharifying enzyme 100 U/g starch, 50 DEG C of reaction 5 h, then boiling water bath heats 20 min termination reactions, makes the starch of unreacted be converted into small molecular sugar;

(5) activated carbon decolorizing

To the granulated active carbon that adds quality product 3% in step (4) products obtained therefrom, 80 DEG C of heating 30 min, filter the sample mix solution obtaining for three times through decolouring repeatedly;

(6) vacuum-drying

By step (5) gained through decolouring sample mix solution vacuumize dry, control drying temperature be 60 DEG C, be 8h time of drying, must contain α-, β-, γ-cyclodextrin contains again the complex loop dextrin product of oligose.

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