CN111410917B - Preparation method of fish skin gelatin-based surfactant - Google Patents

Preparation method of fish skin gelatin-based surfactant Download PDF

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CN111410917B
CN111410917B CN202010373639.XA CN202010373639A CN111410917B CN 111410917 B CN111410917 B CN 111410917B CN 202010373639 A CN202010373639 A CN 202010373639A CN 111410917 B CN111410917 B CN 111410917B
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fish skin
gelatin
skin gelatin
fish
solution
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CN111410917A (en
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涂宗财
刘俊
王辉
李金林
张露
沙小梅
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Jiangxi Normal University
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09H—PREPARATION OF GLUE OR GELATINE
    • C09H3/00—Isolation of glue or gelatine from raw materials, e.g. by extracting, by heating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09H—PREPARATION OF GLUE OR GELATINE
    • C09H1/00—Pretreatment of collagen-containing raw materials for the manufacture of glue
    • C09H1/04—Pretreatment of collagen-containing raw materials for the manufacture of glue of hides, hoofs, or leather scrap
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09H—PREPARATION OF GLUE OR GELATINE
    • C09H5/00—Stabilisation of solutions of glue or gelatine

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Abstract

The invention discloses a preparation method of a fish skin gelatin-based surfactant, which takes fish skin as a raw material, and comprises the steps of carrying out scale removal and degreasing treatment on the fish skin, extracting fish skin gelatin, and treating the fish skin gelatin by adopting ultrasonic pretreatment and glycosylation modification. The method takes the fish skin which is the byproduct of black carp processing as a raw material, and the fish skin gelatin is extracted after alcohol treatment and degreasing; and then high-intensity ultrasonic pretreatment is combined with glycosylation modification of the fish skin gelatin to improve the surface activity of the fish skin gelatin, so that the gelatin-based surfactant is prepared. The method for preparing the fish skin gelatin-based surfactant is simple to operate, is non-toxic and harmless, is easy to realize, and the prepared fish skin gelatin has high emulsifying property and foaming property and has high practical value in liquid foods such as milk, yoghourt and the like.

Description

Preparation method of fish skin gelatin-based surfactant
Technical Field
The invention belongs to the technical field of fish gelatin materials, and particularly relates to a preparation method of a fish skin gelatin-based surfactant.
Background
China is a big fishery country and a big freshwater fish production country, and the freshwater fishery plays an important role in national economy. In 2017, the yield of freshwater fish in China reaches 3123.58 ten thousand tons, and the yield of the freshwater fish accounts for 48.5 percent of the total amount of aquatic products. In recent years, the freshwater fish processing technology and equipment level in China are obviously improved, the product quality is also improved, but the freshwater fish industry still has the problems of low processing rate, unreasonable product structure, lack of comprehensive utilization technology, low achievement conversion rate and the like, the utilization rate of processing byproducts accounting for 40-55% of the weight of fish is less than 20%, the resource waste is serious, the economic loss is caused, and the environment is polluted. The fish skin is one of main byproducts in the processing process of freshwater fish and contains a large amount of nutrients such as collagen and the like.
Fish gelatin is widely used in liquid food products requiring cryopreservation, including milk and yoghurt, and for its use in such products, surface activity, including foaming and emulsifying properties, is the most important factor to be investigated. However, all gelatin materials, including fish gelatin, have relatively low surface activity, particularly emulsifiability and emulsion stability, significantly lower than other surface active materials, such as globulin and acacia. When used alone as an emulsifier, gelatin often produces relatively large sized droplets during homogenization. Therefore, finding a simple and efficient fish skin gelatin-based surfactant would be advantageous for gelatin applications in the food industry.
Disclosure of Invention
The invention provides a preparation method of a fish skin gelatin-based surfactant, which takes fish skin as a raw material, degreases the fish skin, and modifies the fish skin by adopting high-intensity ultrasonic wave and glycosylation to obtain the fish skin gelatin-based surfactant.
Further, the preparation method comprises the following specific steps:
a preparation method of a fish skin gelatin-based surfactant comprises the steps of degreasing fish skin by taking the fish skin as a raw material, and modifying the fish skin by adopting high-intensity ultrasonic waves and glycosylation to obtain the fish skin gelatin-based surfactant.
The preparation method comprises the following specific steps:
(1) pretreatment of raw materials: removing scales from fish skin, scraping surface fat by using a knife, cutting into pieces of 1cm multiplied by 1cm, cleaning, draining, extracting in isopropanol with volume fraction of 15% at 4 ℃ for 24 hours for degreasing, washing with water, draining completely, soaking in sodium chloride solution with mass fraction of 5%, continuously stirring for 12 hours to remove foreign proteins in the fish skin, changing the solution once after 2 hours, rinsing with deionized water, and draining;
(2) preparation of fish skin gelatin: mixing the pretreated fish skin with 0.2mol/L hydrochloric acid solution according to the ratio of 1:5, soaking for 30min, washing with water until the pH value is 4-5, adding deionized water according to the ratio of 1: 4, heating in a water bath at 55 ℃ for 5h, filtering with gauze to obtain gelatin solution, and freeze-drying to obtain the finished product of fish skin gelatin;
(3) ultrasonic treatment: dissolving freeze-dried fish skin gelatin by using distilled water to obtain a fish skin gelatin solution with the mass fraction of the fish skin gelatin being 10%, and adopting a Q700 ultrasonic cell disruption instrument, wherein the working frequency is 20kHz, the working time of ultrasonic pulse is 5s, and the intermittent time is 5s, and the preparation process comprises the following steps: taking 15mL of fish skin gelatin solutionThe solution was filled in a 25mL beaker with an ultrasonic intensity of 120W/cm2Treating in ice bath for 10min, and freeze drying;
(4) and (3) glycosylation modification:
adding 10mg of glucose into 1mL of the fish skin solution after ultrasonic treatment, uniformly mixing, freeze-drying, placing the freeze-dried powder in an incubator to react for 1h at 55 ℃ and 65% relative humidity, immediately placing a centrifuge tube in an ice bath to stop the reaction after the reaction is finished, adding precooled ultrapure water for redissolution after the reaction is finished, and removing redundant sugar by adopting a 10kDa ultrafiltration centrifuge tube to obtain the fish skin gelatin modified by ultrasonic pretreatment and glycosylation.
Preferably, the fish skin is black carp skin.
The invention has the beneficial effects that:
the method takes the fish skin which is the byproduct of black carp processing as a raw material, and the fish skin gelatin is extracted after alcohol treatment and degreasing; and then high-intensity ultrasonic pretreatment is combined with glycosylation modification of the fish skin gelatin to improve the surface activity of the fish skin gelatin, so that the gelatin-based surfactant is prepared. The method for preparing the fish skin gelatin-based surfactant is simple to operate, is non-toxic and harmless, is easy to realize, and the prepared fish skin gelatin has high emulsifying property and foaming property and has high practical value in liquid foods such as milk, yoghourt and the like.
Detailed Description
The following is a detailed description with reference to examples:
example 1
A preparation method of a fish skin gelatin-based surfactant comprises the following specific steps of 1, raw material pretreatment: removing scales from fish skin, scraping surface fat with a knife, cutting into pieces of 1cm multiplied by 1cm, cleaning, draining, extracting in 15% isopropanol with volume fraction at 4 ℃ for 24h for degreasing, washing with water, draining completely, soaking in 5% sodium chloride solution (1:5, m/V) with mass fraction, stirring continuously for 12h to remove foreign proteins in the fish skin, changing the solution once in 2h, rinsing with deionized water, and draining.
2. Preparing black carp skin gelatin: mixing the pretreated fish skin with 0.2mol/L hydrochloric acid solution according to the ratio of 1:5, soaking for 30min, washing with water until the pH value is 4-5, adding deionized water according to the ratio of 1: 4 (m/V), heating in a water bath at 55 ℃ for 5h, filtering with gauze, and freeze-drying to obtain the gelatin solution of the fish skin.
3. Ultrasonic treatment: and dissolving the freeze-dried fish skin gelatin by using distilled water to obtain a fish skin gelatin solution with the mass ratio of the fish skin gelatin being 10%. A Q700 ultrasonic cell disrupter (probe size 1/8 "= 3 mm) was used, the operating frequency was 20kHz, the ultrasonic pulse operating time was 5s, and the rest time was 5 s. The preparation process comprises the following steps: 15mL of fish skin gelatin solution is put into a 25mL beaker, and the ultrasonic intensity is 120W/cm2Treating in ice bath for 10min, and freeze drying.
4. And (3) glycosylation modification:
adding 10mg of glucose into 1mL of the ultrasonically treated fish skin solution, uniformly mixing, and freeze-drying. The freeze-dried powder is placed in an incubator to react for 1h at 55 ℃ and 65% relative humidity (saturated potassium iodide solution), and after the reaction is finished, the centrifuge tube is immediately placed in an ice bath to terminate the reaction. After the reaction is finished, adding pre-cooled ultrapure water for redissolution, and then removing redundant sugar by adopting a 10kDa ultrafiltration centrifugal tube to obtain the fish skin gelatin modified by ultrasonic pretreatment and glycosylation.
Measurement of emulsification characteristics:
the 30 mL of the ultrasonic pretreatment combined with glycosylation modification of fish scale gelatin solution (protein content 1 mg/mL) was mixed with 10 mL of soybean oil, and then dispersed with a disperser (Ultra-Turrax T25, IKA, Germany) at 10,000 rpm for 2 min. Immediately after the end of the dispersion (0 min), 50. mu.L of the emulsion was taken from the bottom of the resulting solution and added to 5mL of a 0.1% SDS solution, mixed well and the absorbance was measured at a wavelength of 500 nm. After 10min, 50. mu.L of the emulsion from the bottom of the resulting solution was added to 5mL of 0.1% SDS solution, mixed well and the absorbance was measured. The light absorption value at 0min is A0And the light absorption value at 10min is A10The calculation formula of emulsification capacity (Emulsifying Stability Index, EAI) and emulsification Stability (Emulsifying Stability Index, ESI) is as follows:
Figure DEST_PATH_IMAGE001
in the formula: a. the0Refers to the absorbance of the emulsion that is rapidly diluted after emulsification; m refers to protein mass concentration (g/mL); a. the10Refers to the absorbance of the emulsion after standing for 10min, Δ t =10 min. Δ A = A0—A10
Measurement of foaming Properties:
the 25mL of the ultrasonically pretreated and glycosylation-modified fish scale gelatin solution (protein content 1 mg/mL) was dispersed with a T25 disperser (Ultra-Turrax T25, IKA, Germany) at 9500 rpm for 2 min, the foamed solution was immediately poured into a graduated cylinder (50 mL), the foam volume of the sample was recorded for determining the Foaming Capacity (FC) of the fish scale gelatin, and the corresponding time was recorded, and the sample volume was again recorded after 30min of standing for determining the Foaming Stability (FS) of the fish scale gelatin.
The FC and FS calculation formulas are as follows:
Figure 247097DEST_PATH_IMAGE002
in the formula: v1And V2Refer to the volume of foam the sample was dispersed at 0 and 30min, respectively.
The experimental result shows that the emulsifying capacity (EAI) and the Emulsifying Stability (ESI) of the fish scale gelatin modified by combining ultrasonic pretreatment and glycosylation are respectively 80 m2The foaming capacity and the foaming stability were 140% and 80%, respectively, for each of 13 min and 13 mg/g.
Example 2
A preparation method of a fish skin gelatin-based surfactant comprises the following specific steps of 1, raw material pretreatment: removing scales from fish skin, scraping surface fat with a knife, cutting into pieces of 1cm multiplied by 1cm, cleaning, draining, extracting in 25% isopropanol by volume at 4 ℃ for 24h for degreasing, washing with water, draining completely, soaking in 8% sodium chloride solution (1:5, m/V) by mass, stirring continuously for 12h to remove foreign proteins in the fish skin, changing the solution once after 2h, rinsing with deionized water, and draining.
2. Preparing black carp skin gelatin: mixing the pretreated fish skin with 0.2mol/L hydrochloric acid solution according to the ratio of 1:5, soaking for 30min, washing with water until the pH value is 4-5, adding deionized water according to the ratio of 1: 4 (m/V), heating in a 65 ℃ water bath for 5h, filtering with gauze, and freeze-drying to obtain the gelatin solution of the fish skin.
3. Ultrasonic treatment: and dissolving the freeze-dried fish skin gelatin by using distilled water to obtain a fish skin gelatin solution with the mass fraction of the fish skin gelatin being 10%. A Q700 ultrasonic cell disrupter (probe size 1/8 "= 3 mm) was used, the operating frequency was 20kHz, the ultrasonic pulse operating time was 5s, and the rest time was 5 s. The preparation process comprises the following steps: 15mL of fish skin gelatin solution is put into a 25mL beaker, and the ultrasonic intensity is 150W/cm2Treating in ice bath for 15 min, and freeze drying.
4. And (3) glycosylation modification:
adding 10mg of glucose into 1mL of the ultrasonically treated fish skin solution, uniformly mixing, and freeze-drying. The freeze-dried powder is placed in an incubator to react for 2 hours at 55 ℃ and 65% relative humidity (saturated potassium iodide solution), and after the reaction is finished, the centrifugal tube is immediately placed in an ice bath to terminate the reaction. After the reaction is finished, adding pre-cooled ultrapure water for redissolution, and then removing redundant sugar by adopting a 10kDa ultrafiltration centrifugal tube to obtain the fish skin gelatin modified by ultrasonic pretreatment and glycosylation.
The emulsifying and foaming properties of the fish skin gelatin were determined as described in the example. The experimental result shows that the emulsifying capacity (EAI) and the Emulsifying Stability (ESI) of the fish skin gelatin modified by combining ultrasonic pretreatment and glycosylation are 82 m respectively2The foaming capacity and the foaming stability were 150% and 85%, respectively, for 14 min and 14 g.
Example 3
This example differs from example 1 in that: omitting the ultrasonic process in step (3), and subjecting the finished gelatin obtained in step (2) to glycosylation treatment according to the data in example 1.
Measuring emulsifying property and foaming property of fish skin gelatinThe method is as described in example one. The experimental results show that the emulsifying capacity (EAI) and the Emulsifying Stability (ESI) of the fish skin gelatin are 56 m respectively2The foaming capacity and the foaming stability were 115% and 65%, respectively, for each of 8 min and 8 min.
Example 4
This example differs from example 1 in that: the sonication process of step (3) and the glycosylation process of step (4) are omitted, as in example 1. The gelatin prepared in step (2) was directly subjected to measurement for the emulsification and foaming properties of fish skin gelatin, as described in example 1. The experimental results show that the emulsifying capacity (EAI) and the Emulsifying Stability (ESI) of the fish skin gelatin are respectively 45 m2The foaming capacity and the foaming stability were 105% and 45%, respectively, for each of the samples,/g and 4 min.
The technical solutions provided by the present invention are described in detail above, and for those skilled in the art, the ideas according to the embodiments of the present invention may be changed in the specific implementation manners and the application ranges, and in summary, the content of the present description should not be construed as limiting the present invention.

Claims (1)

1. The preparation method of the fish skin gelatin-based surfactant is characterized by comprising the following specific steps:
(1) pretreatment of raw materials: removing scales from fish skin, scraping surface fat by using a knife, cutting into pieces of 1cm multiplied by 1cm, cleaning, draining, extracting in isopropanol with volume fraction of 15% at 4 ℃ for 24 hours for degreasing, washing with water, draining completely, soaking in sodium chloride solution with mass fraction of 5%, continuously stirring for 12 hours to remove foreign proteins in the fish skin, changing primary liquid for 2 hours, rinsing with deionized water, and draining;
(2) preparation of fish skin gelatin: mixing and soaking the pretreated fish skin and 0.2mol/L hydrochloric acid solution in a ratio of 1:5 for 30min, washing with water until the pH value is 4-5, adding deionized water in a ratio of 1: 4, heating in a water bath at 55 ℃ for 5h, filtering with gauze to obtain a gelatin solution, and freeze-drying to obtain a finished product of fish skin gelatin;
(3) ultrasonic treatment: dissolving the freeze-dried fish skin gelatin by using distilled water to obtain the fish skin gelatin with the mass fraction of10% fish skin gelatin solution, adopting Q700 ultrasonic wave cell disruption instrument, working frequency is 20kHz, ultrasonic pulse working time is 5s, intermittent time is 5s, and the concrete preparation process is as follows: 15mL of fish skin gelatin solution is put into a 25mL beaker, and the ultrasonic intensity is 120W/cm2Treating in ice bath for 10min, and freeze drying;
(4) and (3) glycosylation modification:
adding 10mg of glucose into 1mL of the fish skin solution after ultrasonic treatment, uniformly mixing, freeze-drying, placing the freeze-dried powder in an incubator to react for 1h at 55 ℃ and 65% relative humidity, immediately placing a centrifuge tube in an ice bath to stop the reaction after the reaction is finished, adding precooled ultrapure water for redissolution after the reaction is finished, and removing redundant sugar by adopting a 10kDa ultrafiltration centrifuge tube to obtain the fish skin gelatin modified by ultrasonic pretreatment and glycosylation.
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CN111345436A (en) * 2020-03-19 2020-06-30 江西师范大学 Preparation method of instant collagen membrane material
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* Cited by examiner, † Cited by third party
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CN101427728A (en) * 2008-12-05 2009-05-13 江苏大学 Method for improving wheat plantule protein capability with supersonic wave
CN108003219A (en) * 2017-12-12 2018-05-08 安徽省寿县丰茂农产品开发有限公司 A kind of can improve cracks rice protein extracting ratio and carries out the method for glycosylation modification to it
CN110938137A (en) * 2019-12-11 2020-03-31 宁波大学 Preparation method of low-fishy-smell fish gelatin protein

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101427728A (en) * 2008-12-05 2009-05-13 江苏大学 Method for improving wheat plantule protein capability with supersonic wave
CN108003219A (en) * 2017-12-12 2018-05-08 安徽省寿县丰茂农产品开发有限公司 A kind of can improve cracks rice protein extracting ratio and carries out the method for glycosylation modification to it
CN110938137A (en) * 2019-12-11 2020-03-31 宁波大学 Preparation method of low-fishy-smell fish gelatin protein

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