CN106149195A - A kind of embedding fish oil and the nano fibrous membrane of ferulic acid and preparation and application simultaneously - Google Patents

Abstract

The invention belongs to the technical field of functional food preparation, and discloses a nanofibrous membrane simultaneously embedding fish oil and ferulic acid, as well as its preparation and application. The preparation method is as follows: dissolving ferulic acid in ethanol, stirring and mixing evenly, adding water and zein fish oil in turn, respectively stirring and mixing uniformly to obtain an electrospinning solution; the obtained electrospinning solution is passed through electrospinning After drying, the nanofibrous film embedding fish oil and ferulic acid is obtained. On the one hand, the nanofiber membrane obtained by the present invention can effectively cover the fishy smell of fish oil, and fully exert the antioxidant performance of ferulic acid to improve the oxidation stability of fish oil; It provides new ideas for the development of functional foods and has broad application prospects in the field of functional foods.

Description

A nanofibrous membrane simultaneously embedding fish oil and ferulic acid and its preparation and application

technical field

The invention belongs to the technical field of functional food preparation, and in particular relates to a nanofiber film simultaneously embedding fish oil and ferulic acid, as well as its preparation and application.

Background technique

With the improvement of living standards, people pay more and more attention to the nutrition and health improvement functions of food. Fish oil is rich in polyunsaturated fatty acids eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), and the intake of EPA and DHA can improve memory and learning, support brain development, etc., so it has good health effect. However, fish oil has a heavy fishy smell, and its taste is difficult to be accepted by most people. Moreover, fish oil is easily oxidized and deteriorates. Therefore, how to cover up the fishy smell of fish oil and improve its antioxidant properties is very important for the development of fish oil functional food. There are still some deficiencies in the traditional fish oil treatment and processing methods, among which nitrogen-filled storage and low-temperature storage are only suitable for large-scale fish oil products; adding antioxidants and deodorants may cause food quality and safety problems; pickling can easily lead to chemical substances The microencapsulation method has a low embedding rate, the oxidation loss of fish oil is relatively large during processing, the wall material and product form used are single, the cost is high, and the characterization of the microcapsules after production cannot be accurately expressed.

Ferulic acid exists in a variety of Chinese herbal medicines, such as Ferulicum, Chuan Shao, Angelica, Cimicifuga, etc. It has obvious physiological activities and is recognized as a natural antioxidant and anti-cancer substance. In recent years, ferulic acid has been widely used in medicine, food, cosmetics and other fields.

Electrospinning (referred to as electrospinning) is a method of using polymer solution or melt under the action of a strong electric field to make the charged polymer solution or melt flow and deform in the electrostatic field, and then evaporate through the solvent or the melt Cooling and solidification to obtain continuous fiber processing technology. Electrospinning is currently the most important method for preparing nanofibers. By adjusting the type of spinning solution and processing technology, fibers with a diameter of 1nm to 1000nm can be obtained. These nanofibers have a high specific surface area and porosity, so they have many potential use. At present, electrospinning is mostly used in the fields of biomaterials, sensor devices, and functional nanotubes, but its application in the food field is less.

Contents of the invention

In order to solve the above shortcomings and deficiencies of the prior art, the primary purpose of the present invention is to provide a method for preparing a nanofibrous membrane that simultaneously embeds fish oil and ferulic acid.

Another object of the present invention is to provide a nanofibrous membrane prepared by the above method that simultaneously embeds fish oil and ferulic acid.

Another object of the present invention is to provide the application of the above-mentioned nanofibrous membrane embedding fish oil and ferulic acid in the field of functional food.

The object of the invention is achieved through the following technical solutions:

A method for preparing a nanofibrous membrane simultaneously embedded with fish oil and ferulic acid, comprising the following preparation steps:

(1) dissolving ferulic acid in ethanol, stirring and mixing;

(2) Add water to the solution of step (1), stir and mix evenly;

(3) Add zein to the solution in step (2), stir and mix evenly at 25-40°C;

(4) Add fish oil to the solution in step (3), stir and mix at 25-40° C. to obtain an electrospinning solution;

(5) Electrospinning and drying the electrospinning solution obtained in step (4) to obtain the nanofibrous membrane simultaneously embedding fish oil and ferulic acid.

Preferably, in the solution of step (1), the mass fraction of ferulic acid added is 1%-3%.

Preferably, the volume ratio of the amount of water added in step (2) to the ethanol added in step (1) is (1-2):8.

Preferably, in the solution in step (3), the mass fraction of zein added is 25%.

Preferably, in the solution in step (4), the mass ratio of the added amount of fish oil to the added zein is 3:10.

Preferably, glycerol with a mass fraction of 1%-5% is also added to the electrospinning solution obtained in step (4).

Preferably, the electrospinning conditions described in step (5) are: the diameter of the needle is 0.6-0.8mm, the distance from the needle to the receiver is 10-20cm, the voltage is 10-20kV, the flow rate of the spinning solution is 0.2-2mL/h, Spinning time 3 ~ 6h.

The invention discloses a nanofibrous membrane simultaneously embedding fish oil and ferulic acid, which is prepared by the above method.

The application of the above-mentioned nanofibrous membrane simultaneously embedding fish oil and ferulic acid in the field of functional food.

The preparation method of the present invention and the resulting product have the following advantages and beneficial effects:

(1) The present invention prepares a nanofibrous membrane loaded with fish oil and ferulic acid simultaneously by electrospinning technology, realizes that the same carrier loads two kinds of active substances, and exerts the synergistic effect of the joint application of active substances. On the one hand, it can effectively cover up the fish oil. Fishy smell, and give full play to the antioxidant properties of ferulic acid to improve the oxidation stability of fish oil; on the other hand, because the product is in the form of nanofibrous membrane, the fish oil is changed from liquid to solid fiber, which provides a great support for the development of fish oil functional products new ideas;

(2) The present invention lays the foundation for the application of electrospinning technology in the production of food, further enriches the types of functional food, and has broad application prospects in the field of functional food.

Description of drawings

Fig. 1 (a), (b), (c) and (d), (e), (f) are the nanofibers of embodiment 1, embodiment 2, embodiment 3 obtained simultaneously embedding fish oil and ferulic acid respectively Scanning electron microscope (SEM) image of the film and its diameter distribution;

Fig. 2 (a), (b), (c) and (d), (e), (f) are the scanning electron microscope (SEM) figure of comparative example 1, comparative example 2, the obtained nanofiber film of comparative example 3 (SEM) and its Diameter distribution map;

Fig. 3 is fish oil (fish oil), ferulic acid (ferulic acid), zein (zein), the nanofibrous membrane (A) obtained in comparative example 3 and the nanofiber film (A) obtained in embodiment 3 simultaneously embedding fish oil and ferulic acid. The infrared spectrogram of fiber film (B);

Figure 4 shows the nanofibrous membrane (A) obtained in Comparative Example 3, the nanofibrous membrane (B) obtained in Example 3 that simultaneously embeds fish oil and ferulic acid, and the blank fish oil stored at 25°C, 45°C and 60°C in the dark for 25°C, respectively. Day-to-day change in peroxide value.

detailed description

The present invention will be further described in detail below in conjunction with the embodiments and the accompanying drawings, but the embodiments of the present invention are not limited thereto.

Example 1

(1) Dissolve 3g ferulic acid in 85mL ethanol, stir well;

(2) add 15mL water in the solution of step (1), make solvent volume ratio ethanol: water=8.5:1.5, stir;

(3) 25 g of zein was dissolved in 100 mL of the above solvent, and stirred in a magnetic stirrer for 0.5 h to obtain a 25% zein solution;

(4) Add a certain amount of fish oil to the solution in step (3) according to the quality of zein: fish oil = 10:3, and magnetically stir for 1 hour at 25-40° C.;

(5) Inhale the solution prepared in (4) into a 5mL syringe as a spinning solution, install a needle with a diameter of 0.6mm, adjust the distance from the needle to the receiver to 14cm, the voltage to 14kv, the flow rate to 0.6mL/h, and the temperature to 27 ℃, 40% humidity, spinning for 4 hours; then vacuum drying at 35 ℃ for 12 hours to obtain a nanofiber membrane embedding fish oil and ferulic acid at the same time.

The SEM image and diameter distribution of the nanofibrous membrane simultaneously embedded with fish oil and ferulic acid obtained in this example are shown in Fig. 1 (a), (d).

Example 2

(1) Dissolve 3g ferulic acid in 85mL ethanol, stir well;

(2) add 15mL water in the solution of step (1), make solvent volume ratio ethanol: water=8.5:1.5, stir;

(3) 25 g of zein was dissolved in 100 mL of the above solvent, and stirred in a magnetic stirrer for 0.5 h to obtain a 25% zein solution;

(4) Add a certain amount of fish oil to the solution in step (3) according to the quality of zein: fish oil = 10:3, and magnetically stir for 1 hour at 25-40° C.;

(5) adding mass fraction in the solution of step (4) is 3% glycerin, stirs;

(6) Inhale the solution prepared in (5) into a 5mL syringe as a spinning solution, install a needle with a diameter of 0.6mm, adjust the distance from the needle to the receiver to 14cm, the voltage to 14kv, the flow rate to 0.6mL/h, and the temperature to 27 ℃, 40% humidity, spinning for 4 hours; then vacuum drying at 35 ℃ for 12 hours to obtain a nanofiber membrane embedding fish oil and ferulic acid at the same time.

The SEM image and diameter distribution of the nanofibrous membrane simultaneously embedded with fish oil and ferulic acid obtained in this example are shown in Fig. 1 (b), (e).

Example 3

(1) Dissolve 3g ferulic acid in 85mL ethanol, stir well;

(2) add 15mL water in the solution of step (1), make solvent volume ratio ethanol: water=8.5:1.5, stir;

(3) 25 g of zein was dissolved in 100 mL of the above solvent, and stirred in a magnetic stirrer for 0.5 h to obtain a 25% zein solution;

(4) Add a certain amount of fish oil to the solution in step (3) according to the quality of zein: fish oil = 10:3, and magnetically stir for 1 hour at 25-40° C.;

(5) adding mass fraction in the solution of step (4) is 3% glycerin, stirs;

(6) Inhale the solution prepared in (5) into a 5mL syringe as a spinning solution, install a needle with a diameter of 0.6mm, and spin as a core spinning solution, and the flow rate is controlled at 0.6mL/h; the shell spinning solution uses ethanol , inhale a 5mL syringe, install a needle with a diameter of 0.6mm, and control the flow rate to 0.2mL/h; adjust the distance from the needle to the receiver to 14cm, the voltage to 14kv, the temperature to 27°C, the humidity to 40%, and spinning for 4h; Vacuum drying at 35° C. for 12 hours yields a nanofiber membrane in which fish oil and ferulic acid are simultaneously embedded.

The SEM image and diameter distribution of the nanofibrous membrane simultaneously embedded with fish oil and ferulic acid obtained in this example are shown in Fig. 1 (c), (f).

Comparative example 1

Compared with Example 1, ferulic acid is not added, and the rest are identical.

The SEM and diameter distribution of the nanofibrous membrane prepared in this comparative example are shown in Fig. 2(a) and (d).

Comparative example 2

Compared with Example 2, ferulic acid is not added, and the rest are identical.

The SEM and diameter distribution of the nanofibrous membrane prepared in this comparative example are shown in Fig. 2(b) and (e).

Comparative example 3

Compared with Example 3, ferulic acid is not added, and the rest are identical.

The SEM and diameter distribution of the nanofibrous membrane prepared in this comparative example are shown in Fig. 2(c), (f).

Characterization and performance testing:

(1) Fish oil, ferulic acid, zein, the nanofibrous membrane (A) obtained in Comparative Example 3 and the nanofibrous membrane (B) that simultaneously embed fish oil and ferulic acid obtained in Example 3 are analyzed together by infrared spectroscopy , and the result is shown in Figure 3.

The interaction between substances can be seen from Figure 3. According to relevant literature, the characteristic absorption peaks of fish oil are the stretching vibration peak of methylene CH at 3013cm- ¹ and the C=O stretching vibration peak of aldehyde group at 1738cm ^-1 ; the characteristic absorption peaks of ferulic acid are 1691cm ^-1 and The C=O stretching vibration peak at 1668cm ^-1 ; the characteristic absorption peaks of zein are the OH stretching vibration peak at 3325cm ^{-1, the C=O stretching vibration peak at 1655cm-1 at} amide Ⅰ, and the 1534cm ^-1 stretching vibration peak with NH in amide II. Through the changes in the peak position and intensity of the infrared spectrum, it can be found whether the interaction between substances occurs. It can be seen from Figure 3 that, compared with the infrared spectrum of ferulic acid, the characteristic absorption peaks of ferulic acid in the nanofibrous membranes simultaneously embedding fish oil and ferulic acid disappeared, indicating that the crystal form of ferulic acid no longer existed. The acid was successfully entrapped; and compared to the infrared spectra of fish oil and zein, the peak positions and peak intensities of the characteristic absorption peaks of fish oil and zein in the two nanofibrous films changed, which indicated that fish oil was entrapped. The embedding was successful and the interaction between the two occurred.

(2) The nanofibrous membrane (A) obtained in Comparative Example 3 and the nanofibrous membrane (B) obtained in Example 3 simultaneously embedding fish oil and ferulic acid were stored at 25°C, 45°C and 60°C in the dark for 25 days, Detect its peroxide value, and use blank fish oil as a control. The detection method of peroxide value refers to the FOX method, which is as follows: immerse 1g nanofibrous membrane in 5mL hexane, centrifuge to get 90μL supernatant and 900μL FOX reaction solution (3.6mmol/L Fe ²⁺ , 125μmol/L xylenol orange , 70μmol/L12NHCl and 4mmol/LBHT dissolved in 90% methanol), after shaking, place at room temperature for 30min, centrifuge at 10000g for 5min, take the supernatant and measure the OD value at 560nm. H ₂ O ₂ was used as standard control. The result is shown in Figure 4.

It can be seen from Figure 4 that the peroxide value of the samples increases significantly with the increase of temperature, and the growth rate of the peroxide value of the three samples is B<A<fish oil. Fitting the data in Figure 4 to the Arrhenius oxidation kinetic model can provide a more comprehensive understanding of its oxidation stability.

Known storage temperature and peroxide value, reaction rate constant (k) and activation energy (Ea) can be calculated by the following formula:

ln(POV/POV ₀ )=kt (1)

k＝k ₀ ×exp(-Ea/RT) (2)

Where: POV is the peroxide value in the sample when the sensory end point is reached, mmol/kg;

POV ₀ is the initial peroxide value of the sample before storage, mmol/kg;

k is the first-order reaction rate constant, day ^-1 ;

k ₀ is the equation constant;

Ea is the activation energy of the reaction, kJ/mol;

R is the gas constant, 8.314J/(mol K);

T is the absolute temperature, K.

According to the formula (2), plot -lnk against the reciprocal of the storage temperature T, and the obtained straight line takes (Ea/R) as the slope, and combined with the _k values obtained at different temperatures, the Ea and k0 values can be obtained.

The data in Figure 4 were fitted with the Arrhenius oxidation kinetic model, and the results are shown in Table 1.

Table 1

It can be seen from Table 1 that the fitting k values of the two nanofibrous membranes are significantly smaller than that of fish oil, and the oxidation activation energy is significantly greater than that of fish oil, indicating that both nanofibrous membranes can significantly improve the oxidation stability of fish oil. The fitting k value of nanofibrous membrane B is smaller and the oxidation activation energy is larger, which indicates that its oxidation stability is stronger than that of nanofibrous membrane A. According to the k value and activation energy Ea in Table 1, the specific oxidation kinetic model can be obtained. The storage temperature is set at room temperature 20°C, and the shelf life can be calculated according to the obtained kinetic model, and the results are shown in Table 2.

Table 2

It can be seen from Table 2 that compared with fish oil, both nanofibrous membranes significantly increased their shelf life at 20°C, indicating that electrospinning embedding fish oil can effectively improve the oxidation stability of fish oil. In addition, the shelf life of nanofiber membrane B is significantly higher than that of nanofiber membrane A, indicating that the blended nanofiber membrane of the present invention that simultaneously entraps fish oil and ferulic acid is significantly superior to fish oil nanofiber membranes in terms of improving the oxidation stability of fish oil .

The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the above-mentioned embodiment, and any other changes, modifications, substitutions, combinations, Simplifications should be equivalent replacement methods, and all are included in the protection scope of the present invention.

Claims (9)

1. the preparation method of the nano fibrous membrane simultaneously embedding fish oil and ferulic acid, it is characterised in that include preparing as follows step Rapid:

(1) ferulic acid is dissolved in ethanol, is uniformly mixed；

(2) in the solution of step (1), add water, be uniformly mixed；

(3) adding zein in the solution of step (2), 25～40 DEG C are uniformly mixed；

(4) adding fish oil in the solution of step (3), 25～40 DEG C are uniformly mixed and obtain electrostatic spinning solution；

(5) by step (4) gained electrostatic spinning solution by being dried after electrostatic spinning, described embedding fish oil and Resina Ferulae simultaneously are obtained The nano fibrous membrane of acid.

The preparation method of a kind of nano fibrous membrane of embedding fish oil and ferulic acid simultaneously the most according to claim 1, it is special Levying and be: in the solution of step (1), the mass fraction that ferulic acid adds is 1%～3%.

The preparation method of a kind of nano fibrous membrane of embedding fish oil and ferulic acid simultaneously the most according to claim 1, it is special Levy and be: the volume ratio that water described in step (2) and ethanol in step (1) add is (1～2): 8.

The preparation method of a kind of nano fibrous membrane of embedding fish oil and ferulic acid simultaneously the most according to claim 1, it is special Levying and be: in the solution of step (3), the mass fraction that zein adds is 25%.

The preparation method of a kind of nano fibrous membrane of embedding fish oil and ferulic acid simultaneously the most according to claim 1, it is special Levying and be: in the solution of step (4), the mass ratio that the addition of fish oil adds with zein is 3:10.

The preparation method of a kind of nano fibrous membrane of embedding fish oil and ferulic acid simultaneously the most according to claim 1, it is special Levy and be: step (4) gained electrostatic spinning solution is additionally added the glycerol that mass fraction is 1%～5%.

The preparation method of a kind of nano fibrous membrane of embedding fish oil and ferulic acid simultaneously the most according to claim 1, it is special Levying and be that described in step (5), the condition of electrostatic spinning is: needle diameter 0.6～0.8mm, the distance of syringe needle to receptor is 10 ～20cm, voltage 10～20kV, spinning solution flow velocity 0.2～2mL/h, spinning time 3～6h.

8. one kind embeds fish oil and the nano fibrous membrane of ferulic acid simultaneously, it is characterised in that: by any one of claim 1～7 Described method prepares.

9. nano fibrous membrane the answering in functional food field of a kind of embedding fish oil and the ferulic acid simultaneously described in claim 8 With.