CN103243140A - 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 kind of preparation method of complex loop dextrin belongs to the cyclodextrin technical field.

Background technology

Since the last century the nineties, starch industry is progressively grown into the national strategy industry, successively is listed in country " 15 ", the Eleventh Five-Year Plan emphasis supports project.The major fields of Dian Fentang industry and study of investment opportunities thereof become hot issue during " 12 ".And W-Gum is topmost kind in the starch, accounts for 80% of world's starch total amount.Carry out the comprehensive utilizating research of W-Gum to complying with " 12 " demand for development, realization grain industry is efficiently rised in value, and is significant.

Cyclodextrin is as an important branch of Dian Fentang; have performances such as good chemical stability, thermostability, anti-enzymolysis, moisture resistance because of it; can with scope extremely widely all kinds of objects form the Subjective and Objective inclusion compound by molecular interaction; thereby object had functions such as shielding, control release, active protection; be widely applied to 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, have great demand, be star's product that a tool has great prospects for development.

The present invention is starting point with cheap W-Gum, utilization ratio with raising starch is target with the service efficiency of improving cyclodextrin, by preparation process condition is explored, prepares and both contains α, beta, gamma-cyclodextrin contains the complex loop dextrin product of oligose again.Compare with traditional cyclodextrin preparation technology, the present invention can adjust the ratio of α, β, three kinds of cyclodextrin of γ according to the needs of using, process controllability is strong, with unconverted for the starch degradation of cyclodextrin be small molecular sugar, both can improve the utilising efficiency of starch greatly, can increase the product solid content again, also improve 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, be raw material with the W-Gum, 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 the complex loop dextrin of oligose again.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 by weighing an amount of W-Gum, quality methyl alcohol such as use to soak into, under 80 ℃, boil 5min, filter, repeatable operation 3 times, thus carry out degreasing;

The degreasing purpose: the fat abstraction of W-Gum can reduce starting temperature, peak temperature, the final temperature of starch, and the gelatinization scope is increased;

(2) starch pasting

Take W-Gum 100g after the degreasing and place the beaker of 400mL, add the water of 200mL, stir, in 62-72 ℃ of water-bath, heat, and continuous stir about 1h, starch slurry by the beginning gelatinization until becoming to stick with paste fully;

(3) add the CGTase enzyme and add the CGTase enzyme

Add CGTase enzyme liquid 400 U/g starch, in 75 ℃ of reaction 1 h down, be cooled to 55 ℃ of the optimal reactive temperatures of enzyme; Add CGTase enzyme liquid 400 U/g starch again, 55 ℃ of reaction 20 h; Heating 20 min termination reactions in the boiling water bath; Be blank with the reaction solution that does not add the CGTase enzyme, 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 ℃ of reaction 5 h, boiling water bath heats 20 min termination reactions then, makes the starch of unreacted be converted into small molecular sugar;

(5) activated carbon decolorizing

Add the granulated active carbon of quality product 3% in step (4) products obtained therefrom, 80 ℃ of heating 30 min filter the sample mix solution that namely gets for three times through decolouring repeatedly;

(6) vacuum-drying

With step (5) gained through the decolouring sample mix solution vacuumize drying, control drying temperature be 60 ℃, be 8h time of drying, namely get contain α-, β-, γ-Huan Hujing contains the complex loop dextrin product of oligose again.

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

Description of drawings

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

Fig. 2 substrate addition is to the influence of compound beta-cyclodextrin yield.

Embodiment

Embodiment 1

Concentration of substrate is to the influence of 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 ℃ of fs temperature; Subordinate phase adds CGTase enzyme amount 400U/g, 55 ℃ of temperature of reaction, other technologies are with reference to above-mentioned cyclodextrin preparation process, discovery is along with the increase of starch substrates concentration in the reaction system, the cyclodextrin transformation efficiency also descends gradually, and the transformation efficiency ratio of three kinds of cyclodextrin the ratio that (see figure 2) shows cyclodextrin mixt in the preparation complex loop dextrin has also taken place to change can be adjusted along with reaction conditions.

Embodiment 2

Complex loop dextrin product quality

During 25 ℃ 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 such as acetic acid then can not hydrolysis complex loop dextrin products, so the chemical property of this product is very stable; This product is at 100 ℃ of heating 30min, and weight does not have considerable change, good thermal stability substantially; This product is 84% o'clock at RH, does not have moisture absorption phenomenon substantially and takes place.

Claims (1)

1. the preparation method of a complex loop dextrin, it is characterized in that: be raw material with the W-Gum, 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, prepare and contain α, beta, gamma-cyclodextrin contains the complex loop dextrin of oligose again; Step is:

(1) degreasing

Take by weighing an amount of W-Gum, quality methyl alcohol such as use to soak into, under 80 ℃, boil 5min, filter, repeatable operation 3 times, thus carry out degreasing;

(2) gelatinization

Take W-Gum 100g after the degreasing and place the beaker of 400mL, add the water of 200mL, stir, in 62-72 ℃ of water-bath, heat, and constantly stir 1h, starch slurry by the beginning gelatinization until becoming to stick with paste fully;

(3) add the CGTase enzyme and add the CGTase enzyme

Add CGTase enzyme liquid 400 U/g starch, in 75 ℃ of reaction 1 h down, be cooled to 55 ℃ of the optimal reactive temperatures of enzyme; Add CGTase enzyme liquid 400 U/g starch again, 55 ℃ of reaction 20 h; Heating 20 min termination reactions in the boiling water bath; Be blank with the reaction solution that does not add the CGTase enzyme, 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 ℃ of reaction 5 h, boiling water bath heats 20 min termination reactions then, makes the starch of unreacted be converted into small molecular sugar;

(5) activated carbon decolorizing

Add the granulated active carbon of quality product 3% in step (4) products obtained therefrom, 80 ℃ of heating 30 min filter the sample mix solution that namely gets for three times through decolouring repeatedly;

(6) vacuum-drying

With step (5) gained through the decolouring sample mix solution vacuumize drying, control drying temperature be 60 ℃, be 8h time of drying, namely get contain α-, β-, γ-Huan Hujing contains the complex loop dextrin product of oligose again.

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