TWI631905B - Method for manufacturing chitin nanofibers-sodium chloride solution - Google Patents

Abstract

The present invention provides a method for producing a chitin nanofiber sodium chloride solution, which is capable of structurally recombining a general chitin, thereby producing a chitin nanofiber having a diameter significantly smaller than that of a general chitin, and The experimental results show that the diameter and interface potential of the final chitin nanofibers are different depending on the ultrasonic treatment time used; after that, 0.3% chlorination is added to the chitin nanofiber solution. Sodium is formulated into a chitin nanofiber sodium chloride solution; however, the experimental data also shows that the various chitin nanofiber sodium chloride solutions prepared by the present invention are compared with 0.3% of the general chlorine. Control salt exhibits a high salty perception and has the potential to be used in low sodium foods.

Description

Method for producing chitin nanofiber sodium chloride solution

The invention relates to the technical field related to enhancing the salty taste of sodium chloride, in particular to a method for preparing a chitin nano-fiber sodium chloride solution by structurally recombining general chitin and then adding sodium chloride. .

With the changes in lifestyle and diet, the age of hypertensive patients has been decreasing year by year. Compared with other malignant diseases, high blood pressure on the human body is more moderate, and there is no obvious symptoms in the initial stage, so it is easily overlooked. However, if not properly controlled, high blood pressure can cause other major diseases, such as stroke, heart disease, kidney failure, and eye lesions. Therefore, it is necessary to reduce the intake of sodium salt in daily life, and it is also the goal of the food industry to work together.

At present, the sodium reduction method used in the food manufacturing process by the food industry is mainly divided into the following four types: (1) using salt substitutes, (2) using taste enhancer, and (3) modifying chlorination. The structure of sodium (ie, reducing the grain size of sodium chloride, increasing the reaction surface area of sodium chloride, rapidly increasing the sodium concentration, thereby improving the salty taste perception), and (4) gradually reducing the salt through a long period of time. It is not perceived by consumers that the flavor and quality of the product are different. Among them, the salt, such as potassium chloride, can also impart a salty taste to the food, but a high content of potassium chloride produces a significant bitterness and a metallic taste; therefore, if potassium chloride is used in a food having a mild taste, Users will notice the bitterness and metallic taste. Further, the flavor enhancer (for example, sodium glutamate, generally referred to as monosodium glutamate) has an effect of enhancing the flavor of the food by sensitizing the taste sensation in the taste bud cells by virtue of the umami taste. However, excessive intake of MSG can cause health problems such as hyperactivity and headache, so manufacturers must appropriately limit the amount of MSG added to the product.

The results show that the diameter of chitin nanofibers produced by different ultrasonic treatments will decrease with the increase of treatment time, and the increase of treatment time will make the diameter distribution of chitin nanofibers smaller; in general, Smaller diameter nanofibers with smaller diameters have more amine groups (positive charges) exposed on the surface of the fiber bundle, so they have stronger ability to adsorb chloride ions (negative charges) and increase the chance of sodium ions being freed in solution. To increase the salty perception. Therefore, the inventors of the present invention have vigorously researched and developed a method for modifying the structure of chitin, and finally developed a method for producing a chitin nanofiber sodium chloride solution of the present invention; wherein the manufacturing method is by nanometer. The fibrillation method reorganizes the chitin structure, enhances the ability to adsorb chloride ions (negative charge), and has the ability to enhance the salty taste of the solution. In addition, the mixed solution is also free amine exposed on the surface of chitin nanofibers. The ability to reduce the astringency of the solution is less.

The main object of the present invention is to provide a method for producing a chitin nanofiber sodium chloride solution, which is capable of structurally recombining a general chitin and preparing a chitin nanofiber, and the experimental results show that Depending on the processing time of the ultrasonic waves used, the diameter and interface potential of the final chitin nanofibers will be different; after that, 0.3% sodium chloride is added to the chitin nanofiber solution to prepare Chitin nanofiber sodium chloride solution; however, the experimental data also show that the various chitin nanofiber sodium chloride solutions prepared by the present invention are compared with the general 0.3% sodium chloride. High salty perception and potential to be applied to low sodium foods.

Therefore, in order to achieve the above object of the present invention, the inventors of the present invention have proposed a method for producing a chitin nanofiber sodium chloride solution, which comprises the following steps:

(1) preparing a beta chitin and pouring the chitin into a deionized water to obtain a chitin suspension solution; (2) using an ultrasonic breaker to the chitin suspension solution Performing ultrasonic oscillation to destroy the hydrogen bond of the chitin to complete a nanofibrosis process; and (3) preparing sodium chloride and pouring the sodium chloride into the finished nanofiber In the chitin suspension solution of the chemical process, a mixed solution is obtained while continuously stirring the sodium chloride.

In the above method for producing a chitin nanofiber sodium chloride solution, preferably, the third chitin nanofiber sodium chloride solution (CNF60) has the best effect of enhancing salty taste.

In order to more clearly describe a method for producing a chitin nanofiber sodium chloride solution of the present invention, a preferred embodiment of the present invention will be described in detail below with reference to the drawings.

First, Fig. 1 is a scanning electron microscope image of a general β chitin. Among them, the camera image of Fig. 1 is obtained by taking a general β chitin under a scanning electron microscope. As shown in the figure, when β-chitin is generally not treated with nanofibers, its structure is elongated.

Please refer to FIG. 2, which is a flow chart of the steps of the method for producing the chitin nanofiber sodium chloride solution of the present invention. As shown in FIG. 2, the manufacturing method of the chitin nanofiber sodium chloride solution of the present invention comprises the following steps: Step (S01): preparing a β chitin and pouring the chitin into a deionized water. In the step of obtaining a chitin suspension solution; step (S02): ultrasonically oscillating the chitin suspension solution by using an ultrasonic breaker to destroy the hydrogen bond of the chitin to complete the a rice fiberizing process; and a step (S03): preparing sodium chloride, and pouring the sodium chloride into the chitin suspension solution for completing the nanofibrillation process, thereby continuously stirring the chlorination In the case of sodium, a mixed solution is obtained.

Here, it must be additionally noted that, in the step (S02), a power of the ultrasonic breaker is 20 kHz, 200 W; and, in the step (2), one of the ultrasonic breakers The processing time can be 30 minutes, 45 minutes, or 60 minutes. At the same time, a set pulse time of the ultrasonic breaker is set to act for 9 seconds to stop for 4 seconds. Thereafter, a centrifugal speed is performed by a centrifuge. After setting to 12,000 rpm and running for 20 minutes, the supernatant was taken to obtain a first chitin nanofiber solution (CNF30), a second chitin nanofiber solution (CNF45), and a third. Butyl nanofiber solution (CNF60).

Continuing, the data of the concentration of the chitin nanofibers and the degree of deacetylation of 20 kHz, 200 W ultrasonic treatment for 30, 45, and 60 minutes are compiled in Table (1). Chitin described in Table (1) is chitin without ultrasonic treatment, CNF30 is the first chitin nanofiber solution treated by ultrasonic for 30 minutes, and CNF45 is treated by ultrasonic for 45 minutes. The chitin nanofiber solution and CNF60 are the third chitin nanofiber solution which has been ultrasonically treated for 60 minutes. From Table (1), it can be found that the nanofiber concentrations of ultrasonic treatment at 30, 45, and 60 minutes were 0.28 mg/mL, 0.33 mg/mL, and 0.29 mg/mL, respectively, indicating that the ultrasonic treatment was performed at different times. The difference in concentration of rice fiber is small. Next, the deacetylation degree of CNF30, CNF45, and CNF60 was determined by infrared spectroscopy, and the degree of deacetylation was changed from 23.15% to 21.59%, 22.30%, and 20.54%, respectively, but there was no statistically significant difference. Table I) ^a If the letters on the data are different, there is a statistically significant difference (p < 0.05).

Next, 20 kHz, 200 W ultrasonic treatment of 30, 45, 60 minutes of chitin nanofibers were made into a transmission electron microscope sample, and the appearance of the CNF30, CNF45 and CNF60 was taken by a transmission electron microscope. Figures 3, 4, and 5, respectively, are then calculated using the image J software and listed in Table (2). From Table (2), it can be found that the diameters of CNF30, CNF45, and CNF60 are 9.34±2.58 nm, 5.61±1.49 nm, and 5.14±1.46 nm, respectively, indicating that the diameter decreases as the ultrasonic processing time increases. Table II) ^{If a~b} is different in the data superscript, there is a statistically significant difference (p < 0.05).

Please refer to FIG. 3, which is a transmission electron microscope image of CNF30. The image of FIG. 2 is obtained by photographing the CNF 30 using a transmission electron microscope. Further, it can be found from FIG. 2 that the above steps (S01) to (S02) are ultrasonically treating the chitin suspension solution for 30 minutes; thus, after the chitin suspension solution is subjected to nanofibrillation, The structure is reorganized and a first chitin nanofiber solution is formed for the purpose of modifying the chitin structure. Obviously, after structural modification, the diameter of the chitin nanofibers is smaller than that of general chitin.

Please refer to FIG. 4, which is a transmission electron microscope image of CNF45. The image of FIG. 3 is obtained by photographing the CNF 45 using a transmission electron microscope. Further, it can be found from FIG. 3 that the chitin suspension solution is treated in 45 minutes; thus, when the chitin suspension solution undergoes nanofibrillation, its structure is reorganized and forms a second batch. The nanofiber solution is used to modify the structure of chitin. Obviously, after structural modification, the diameter of the chitin nanofibers is smaller than that of general chitin.

Please refer to FIG. 5, which is a transmission electron microscope image of CNF60. The image of FIG. 4 is obtained by photographing the CNF 60 using a transmission electron microscope. Further, it can be found from FIG. 4 that the chitin suspension solution is treated in 60 minutes; thus, when the chitin suspension solution undergoes nanofibrillation, the structure is recombined and forms a third batch. The nanofiber solution is used to modify the structure of chitin. Obviously, after structural modification, the diameter of the chitin nanofibers is smaller than that of general chitin.

Herein, the method for producing the chitin nanofiber sodium chloride solution, wherein the step (1) comprises the following detailed steps: Step (S011): taking a squid cartilage Drying in an oven, pulverizing the dried squid cartilage with a pulverizer to obtain a squid cartilage powder; and step (S012): removing the lipoprotein from the squid cartilage powder at room temperature, and then performing Treatment with a strong base, after which the β chitin is obtained.

Further, the step (S012) comprises the following detailed steps: Step (S121): Prepare 50 grams of the salmon cartilage powder, and add the salmon cartilage powder to a 500 mL testosterone solution (0.5%) and Stirring for 24 hours to complete a lipoprotein removal process; Step (S122): adding the salmon cartilage powder that completes the lipoprotein removal process to 500 mL of sodium hydroxide solution, and obtaining the said after stirring for 24 hours Beta chitin.

Next, the concentration of CNF30, CNF45, and CNF60 at 0.3, 0.15, and 0.075 mg/mL were added to 0.01%, 0.05%, and 0.1% sodium chloride for interfacial potential analysis, and the data were compiled in Table (3). From Table (3), it can be found that CNF30, CNF45, and CNF60 have a decrease in interface potential after the addition of sodium chloride. And CNF30, CNF45, and CNF60, after adding 0.01% sodium chloride, the interfacial potential of CNF30, CNF45, and CNF60 will decrease from 30~37 mV to 20~25 mV; and, after adding 0.05% sodium chloride, CNF30, The interface potential of CNF45 and CNF60 will decrease to 17~21 mV; the interface potential of CNF30, CNF45 and CNF60 will decrease to 13~16 mV after adding 0.1% sodium chloride. From this result, it can be seen that the sodium chitin nanofiber sodium chloride solution having a sodium chloride concentration of 0.01% to 0.1% causes the interface potential to decrease as the salt concentration increases. Table (3)

Finally, the inventor of the case completed the salty taste scoring experiment with the salty taste score method. In the experiment, 20 untrained people were used to taste 0.3 mg/mL, 0.15 mg/mL and 0.075 mg/mL chitin nanofiber solutions (diluted by 1, 2, 4 times, respectively) and 0.3% respectively. Sodium chloride is formulated into a chitin nanofiber sodium chloride solution, and then subjected to a salty taste score; wherein the scoring method is 7 points: 1 point means no taste, 2 points means very salty, 3 points means not salty, 4 points means moderate saltiness, 5 points means a bit salty, 6 points means salty, and 7 points means very salty. As shown in Table (4), the salty taste score statistics show that the concentration of CNF30, CNF45, and CNF60 prepared by the present invention is 0.075 mg/mL, 0.15 mg/mL, and 0.3 mg/mL, and the concentration of sodium chloride added is 0.3% of CNF30, CNF45, and CNF60, 18 different concentrations of CNF30, CNF45, and CNF60 exhibited higher salty taste perception than 0.3% of normal sodium chloride (Control Salt). Among them, the effect of enhancing the salty taste with CNF60 is the best. In terms of astringency, it can be found that the chitin suspension solution without adding sodium chloride has a strong astringency, and the astringency is decreased after the addition of sodium chloride. This result can prove that the chitin nanofibers are positively charged. The amine-based electrostatic adsorption of negatively charged chloride ions increases the chance that sodium ions will be freed in solution, increasing salty taste, and because the amine groups on the molecular chain of chitin nanofibers adsorb chloride ions, they are exposed to chitin. The surface of the nanofibers has less free amine groups, which reduces the astringency. Table (4) ^A~c At the same sample concentration, if the letters on the data superscript are different, there is a statistically significant difference (p < 0.05).

Thus, the above description has completely and clearly disclosed the method for producing the chitin nanofiber sodium chloride solution of the present invention, and, through the above, we can know that the present invention has the following advantages: the present invention The method for producing the nanometer cellulose sodium chloride solution is capable of structurally recombining the general chitin, thereby producing a solution having a diameter significantly smaller than that of a general chitin solution. Moreover, the experimental results show that the diameter and interface potential of the finally prepared chitin nanofiber sodium chloride solution are different depending on the ultrasonic treatment time used; however, the experimental data also show the present invention. The various chitin nanofiber sodium chloride solutions obtained have higher salty taste perception than the general 0.3% sodium chloride control, and have certain potential for application in low sodium foods. Among them.

It is to be understood that the foregoing detailed description of the embodiments of the present invention is not intended to Both should be included in the scope of the patent in this case.

<present invention>
S01~S03‧‧‧ method steps

1 is a scanning electron microscope image of a general β chitin; FIG. 2 is a flow chart of a method for producing a chitin nanofiber sodium chloride solution of the present invention; FIG. 3 is a transmission electron microscope of CNF30. Fig. 4 is a transmission electron microscope image of CNF45; and Fig. 5 is a transmission electron microscope image of CNF60.

Claims (7)

A method for producing a chitin nanofiber sodium chloride solution comprises the steps of: (1) preparing a beta chitin and pouring the chitin into a deionized water to obtain a few a suspension solution; (2) ultrasonically oscillating the chitin suspension solution with an ultrasonic breaker to destroy hydrogen bonds between the chitin molecules to complete a nanofibrillation process; and (3) Preparing sodium chloride, and pouring the sodium chloride into the chitin suspension solution for completing the nanofibrillation process, thereby obtaining a specific chlorine while continuously stirring the sodium chloride A sodium butadiene fiber sodium chloride solution having a sodium concentration, and the specific sodium chloride concentration is 0.01% to 0.3%. The method for producing a chitin nanofiber sodium chloride solution according to claim 1, wherein the step (1) comprises the following detailed steps: (11) taking a squid cartilage and drying it in an oven. Then, the dried squid cartilage is pulverized by a pulverizer to obtain a squid cartilage powder; and (12) the lipoprotein is removed from the squid cartilage powder at room temperature, and then subjected to a strong alkali treatment, and then The beta chitin is obtained. The method for producing a chitin nanofiber sodium chloride solution according to claim 2, wherein the step (12) comprises the following detailed steps: (121) Prepare 50 g of the squid cartilage powder, and add the squid cartilage powder to 500 mL of a 0.5% concentration testosterone solution and stir for 24 hours to complete a lipoprotein removal process; and (122) will be completed The salmon cartilage powder of the lipoprotein removal process was added to 500 mL of a sodium hydroxide solution, and the β chitin was obtained after stirring for 24 hours. The method for producing a chitin nanofiber sodium chloride solution according to claim 1, wherein the chitin suspension solution has a specific volume, and the specific volume is 150 ml. The method for producing a chitin nanofiber sodium chloride solution according to claim 1, wherein in the step (2), a power of the ultrasonic breaker is 20 kHz, 200 W; In the step (2), a processing time of the ultrasonic breaker can be 30 minutes, 45 minutes, or 60 minutes, and a set pulse time of the ultrasonic breaker is set to act for 9 seconds to stop 4 Second, after that, a centrifugation speed is performed in a centrifuge, and the supernatant is set to 12,000 rpm for 20 minutes, and then the supernatant is taken to obtain a first chitin nanofiber solution (CNF30) and a second number. Butyl nanofiber solution (CNF45) and a third chitin nanofiber solution (CNF60), wherein the first chitin nanofiber solution (CNF30) and the second chitin nanofiber solution (CNF45), and the third chitin nanofiber solution (CNF60) respectively have a deacetylation degree, and the deacetylation degree is 21.59%, 22.30%, and 20.54%, respectively. The method for producing a chitin nanofiber sodium chloride solution according to claim 5, wherein the first chitin nanofiber solution (CNF30) and the second chitin nanofiber solution are used. (CNF45) and the third chitin nanofiber solution (CNF60) have an interface potential, and the interface potentials are 33.10 to 37.30 mV, 30.17 to 36.20 mV, and 31.03 to 32.43 mV, respectively. The method for producing a chitin nanofiber sodium chloride solution according to claim 5, wherein the first chitin nanofiber solution (CNF30) and the second chitin nanofiber solution are used. (CNF45), and the third chitin nanofiber solution (CNF60) have a diameter, respectively, and the diameters are 9.34±2.58 nm, 5.61±1.49 nm, and 5.14±1.46 nm, respectively.