CN107581461B - Preparation method of high-whiteness Peru squid skin gelatin - Google Patents
Preparation method of high-whiteness Peru squid skin gelatin Download PDFInfo
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- CN107581461B CN107581461B CN201710877641.9A CN201710877641A CN107581461B CN 107581461 B CN107581461 B CN 107581461B CN 201710877641 A CN201710877641 A CN 201710877641A CN 107581461 B CN107581461 B CN 107581461B
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Abstract
The invention relates to a preparation method of gelatin, and particularly provides a preparation method of high-whiteness Peru squid skin gelatin, which is characterized by comprising the following steps: (1) pretreating raw materials; (2) degreasing and removing foreign proteins; (3) and (3) decoloring: putting the squid skin washed to be neutral in Na2CO3Stirring the solution at room temperature for 1.5-2h until Na2CO3Changing the solution every 15-25min until the solution color is light to constant; (4) demineralizing to neutrality; (5) extracting gelatin; (6) filtering and drying. The preparation method of the high-whiteness Peru squid skin gelatin provided by the invention has the advantages of simple process control, easy operation, high decoloring efficiency and low gelatin loss rate; the prepared gelatin has light color and higher whiteness, and the economic value of the gelatin is greatly improved; safe and nontoxic, low production cost and easy industrial production.
Description
Technical Field
The invention relates to a preparation method of gelatin, and in particular relates to a preparation method of high-whiteness Peru squid skin gelatin.
Background
Gelatin (Gelatin) is a soluble natural high-molecular polypeptide polymer, and is the main product of collagen after mild and irreversible breakage. Due to the unique physical and chemical properties and functionality, the product can be used as a gelling agent, a thickening agent, an emulsifier, a filler, a stabilizer, an adhesive, a foaming agent, a clarifying agent and the like, and is widely applied to the fields of chemical industry, food, medicine, make-up and the like. The squid resources in China are rich, the squid skin accounts for about 10 percent of byproducts in the deep processing process of the squid, the current extraction process of the squid skin gelatin comprises an alkali extraction method, an acid extraction method, a hot water extraction method and an enzyme extraction method, but because the squid skin contains a certain amount of pigment, the extracted gelatin is generally dark red or pink, so the application of the gelatin is greatly limited. Therefore, the squid skin must be decolorized to improve the whiteness of the product.
The existing decoloring treatment methods which are applied in production mostly are activated carbon adsorption and hydrogen peroxide decoloring, but the operation is complicated, the time is long, the decoloring effect is not ideal, and the gelatin is easy to be mixed with activated carbon and is difficult to remove, so that the further processing of the gelatin is influenced.
For example, chinese patent publication No. CN103060407A, published 2013, 4 and 24, discloses a process for preparing high-transparency squid skin collagen. According to the method, squid skin which is one of marine product processing wastes is used as a raw material, and the collagen with light color is prepared by adopting a decoloring method of combining EDTA (ethylene diamine tetraacetic acid) and sodium polyphosphate chelation with hydrogen peroxide. The disadvantages are as follows: the utilization rate of hydrogen peroxide in the decoloring process is low, the decoloring rate is about 82%, and the prepared collagen is light pink and is not beneficial to production and application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the preparation method of the Peru squid skin gelatin with high whiteness, and the prepared squid skin gelatin has high whiteness, wide application range and high economic value.
The technical scheme adopted by the invention is as follows: a preparation method of high-whiteness Peru squid skin gelatin comprises the following steps:
(1) pretreatment of raw materials: washing squid skin with distilled water, removing surface impurities, cutting into pieces, and freeze-drying for 72 hours for later use;
(2) degreasing and removing foreign proteins: placing the dried squid skin into 0.05-0.10mol/L NaOH solution, magnetically stirring for 3-5h at room temperature, and finally washing the solution to be neutral by using distilled water;
the method has the advantages of degreasing by adopting NaOH solution, safety, no toxicity, high degreasing efficiency, low cost, more thorough protein removal and contribution to the subsequent extraction of gelatin.
(3) And (3) decoloring: putting the squid skin washed to be neutral in Na2CO3Stirring the solution at room temperature for 1.5-2h until Na2CO3Changing the solution every 15-25min until the solution color is light to constant; by using Na2CO3After the first decolorization of the solution is finished, adjusting the pH value of the solution to 8.0, adding a complexing agent, stirring for 11-13h until the color of the solution is nearly white, and then washing the squid skin with distilled water to be neutral; wherein the complexing agent is ethylenediamine tetraacetic acid;
(4) demineralization: placing the decolorized squid skin into 0.05-0.10mol/L HCl solution, magnetically stirring at room temperature for 55-65min, changing liquid every 25-35min, and washing the solution with distilled water to neutrality;
(5) gelatin extraction: adding the squid skin into distilled water according to the material-liquid ratio of 1: 20-40, and placing the mixture in a constant-temperature water bath kettle to extract gelatin; the method also comprises a deodorization step after the gelatin is extracted, and specifically comprises the following steps: soaking the squid skin gelatin extract in 4-5 wt% trehalose solution at room temperature for 30-40 min.
After being soaked in the trehalose solution, the fishy smell of the squid skin gelatin extract almost disappears; in addition, the trehalose belongs to low-calorie polysaccharide, and can be added into squid skin gelatin extract to improve the gel strength of gelatin.
(6) Filtering and drying: and (3) cooling the deodorized gelatin solution at room temperature for 30min, filtering with 150-mesh 200-mesh gauze to obtain a gelatin extract, and freeze-drying the gelatin extract for 72h to obtain the high-whiteness Peru squid skin gelatin finished product. The squid skin gelatin prepared by freeze drying has good sense and high yield.
Further, changing the alkali liquor once every 30-60min in the process of magnetic stirring in the step (2).
Further, in the step (2), the amount of the NaOH solution per 1g of the squid skin is 10-20 mL.
Further, in the step (3), Na2CO3The concentration of the solution is 0.4-0.6 mol/L.
Further, in the step (3), after adding the complexing agent for decoloring, the method further comprises the following steps: heating the solution to 45-55 deg.C, adding 7.5-8.5 wt% of acidified attapulgite clay, and stirring for 55-65min to complete decolorization. Na (Na)2CO3The EDTA is matched with the attapulgite clay for decoloring, the process control is simple, the operation is easy, the decoloring efficiency is high, the decoloring rate reaches about 95 percent, and the gelatin loss rate is low; in addition, the squid skin has serious fishy smell, and the attapulgite clay can not only be decolorized, but also be deodorized, so that the prepared squid skin gelatin not only has good color, but also can partially deodorize.
Further, the concentration of the complexing agent is 0.2-0.4 mol/L.
Further, in the step (4), the amount of the HCl solution per 1g of the squid skin is 10-20 mL.
Further, in the step (5), gelatin is extracted by hot water, the temperature is increased by 5 ℃ every 1h by taking 55 ℃ as an initial extraction temperature, and the extraction temperature is increased to 70 ℃ by hot water extraction for 3 h.
The invention has the beneficial effects that: the preparation method of the high-whiteness Peru squid skin gelatin provided by the invention has the advantages that the process control is simple, the operation is easy, the decoloring efficiency is high, the gelatin loss rate is low, the prepared gelatin has higher whiteness, stable color and luster, and good stability, and is not easy to fade; the gelatin gel obtained by extraction has high strength; the prepared gelatin has light color and higher whiteness, and the economic value of the gelatin is greatly improved; safe and nontoxic, low production cost and easy industrial production.
Detailed Description
The present invention will be further illustrated with reference to the following specific embodiments.
Example (b):
the embodiment provides a preparation method of high-whiteness Peru squid skin gelatin, which comprises the following steps:
(1) pretreatment of raw materials: washing squid skin with distilled water, removing surface impurities, cutting into pieces of 1 × 1cm, and freeze-drying for 72 hr;
(2) degreasing and removing foreign proteins: placing the dried squid skin into 0.05-0.10mol/L NaOH solution, magnetically stirring for 3-5h at room temperature, changing alkali liquor every 30-60min during the magnetic stirring process, and finally washing the solution to be neutral (pH 7.0-7.5) by using distilled water; wherein the amount of NaOH solution per 1g of squid skin is 10-20 mL.
The method has the advantages of degreasing by adopting NaOH solution, safety, no toxicity, high degreasing efficiency, low cost, more thorough protein removal and contribution to the subsequent extraction of gelatin.
(3) And (3) decoloring: placing the squid skin washed to be neutral in Na with the concentration of 0.4-0.6mol/L2CO3Solutions of
(1) Stirring at room temperature (20-25 deg.C) for 1.5-2h until Na2CO3Changing the solution every 15-25min until the solution color is light to constant to complete the first decolorization; after the first decolorization is finished, adjusting the pH value of the solution to 8.0, adding a complexing agent with the concentration of 0.2-0.4mol/L, stirring for 11-13h until the color of the solution is nearly white, and then cleaning the squid skin solution with distilled water for 4-5 times to be neutral. Then heating the solution to 45-55 ℃, adding 7.5-8.5% of acidified attapulgite clay by mass, and stirring for 55-65min to complete decolorization.
(4) Demineralization: placing the decolorized squid skin in 0.05-0.10mol/L HCl solution, magnetically stirring at room temperature (20-25 deg.C) for 55-65min, changing the solution every 25-35min, and washing the solution with distilled water to neutral (pH 6.5-7.0); the dosage of HCl solution for every 1g of squid skin is 10-20 mL.
(5) Gelatin extraction: adding the squid skin into distilled water according to the material-liquid ratio of 1: 20-40, and placing the mixture in a constant-temperature water bath kettle to extract gelatin; extracting gelatin with hot water at 55 deg.C for 5 deg.C every 1 hr until the extraction temperature is 70 deg.C.
(6) Soaking the squid skin gelatin extract in 4-5 wt% trehalose solution at room temperature for 30-40 min.
(7) Filtering and drying: and (3) cooling the deodorized gelatin solution at room temperature for 30min, filtering with 150-mesh 200-mesh gauze to obtain a gelatin extract, and freeze-drying the gelatin extract for 72h to obtain the high-whiteness Peru squid skin gelatin finished product. The drying method is freeze drying. The squid skin gelatin prepared by freeze drying has good sense and high yield.
Using distilled water as a blank, respectively measuring the color difference values of the gelatin extraction stock solution and the gelatin extraction solution by using a color difference meter, and sequentially marking as delta E1 and delta E2, wherein the calculation formula of the decolorization rate is as follows: the decolorization ratio was (Δ E1- Δ E2) ÷ Δ E1 × 100%, and the decolorization ratio was (15.01-0.72) ÷ 15.01 × 100% ═ 95.2%.
The above examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims and any design similar or equivalent to the scope of the invention.
Claims (6)
1. A preparation method of high-whiteness Peru squid skin gelatin is characterized by comprising the following steps:
(1) pretreatment of raw materials: washing squid skin with distilled water, removing surface impurities, cutting into pieces, and freeze-drying for 72 hours for later use;
(2) degreasing and removing foreign proteins: placing the dried squid skin into 0.05-0.10mol/L NaOH solution, magnetically stirring for 3-5h at room temperature, and finally washing the solution to be neutral by using distilled water;
(3) and (3) decoloring: putting the squid skin washed to be neutral in Na2CO3Stirring the solution at room temperature for 1.5-2h, and changing the solution every 15-25 min; by using Na2CO3After the first decolorization of the solution is finished, adjusting the pH value of the solution to 8.0, adding a complexing agent, stirring for 11-13h, heating the solution to 45-55 ℃, adding 7.5-8.5 mass percent of acidified attapulgite clay, and stirring for 55-65min to finish decolorization; then washing the squid skin with distilled water to be neutral; wherein the complexing agent is ethylenediamine tetraacetic acid;
(4) demineralization: placing the decolorized squid skin into 0.05-0.10mol/L HCl solution, magnetically stirring at room temperature for 55-65min, changing liquid every 25-35min, and washing the solution with distilled water to neutrality;
(5) gelatin extraction: adding the squid skin into distilled water according to the material-liquid ratio of 1: 20-40, and placing the mixture in a constant-temperature water bath kettle to extract gelatin; the method also comprises a deodorization step after the gelatin is extracted, and specifically comprises the following steps: soaking the squid skin gelatin extract in 4-5 wt% trehalose solution at room temperature for 30-40 min;
(6) filtering and drying: and (3) cooling the deodorized gelatin solution at room temperature for 30min, filtering with 150-mesh 200-mesh gauze to obtain a gelatin extract, and freeze-drying the gelatin extract for 72h to obtain the high-whiteness Peru squid skin gelatin finished product.
2. The method of claim 1, wherein: and (3) changing the alkali liquor every 30-60min in the process of magnetic stirring in the step (2).
3. The method of claim 1, wherein: in the step (2), the amount of NaOH solution per 1g of squid skin is 10-20 mL.
4. The method of claim 1, wherein: in the step (3), Na2CO3The concentration of the solution is 0.4-0.6 mol/L.
5. The method of claim 1, wherein: the concentration of the complexing agent is 0.2-0.4 mol/L.
6. The method of claim 1, wherein: in the step (4), the dosage of HCl solution per 1g of squid skin is 10-20 mL.
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