Method for improving oxidation resistance of caramel color of powder produced by ammonia process

Abstract

The invention discloses a method for improving oxidation resistance of an ammonia process powder caramel color. The method specifically comprises the following steps: (1) carrying out pretreatment on the ammonia process powder caramel color, and carrying out superfine grinding to 100-200 meshes; (2) putting the powder caramel color obtained by the ammonia process into a reaction container, and introducing nitrogen; (3) under the protection of nitrogen, carrying out ultrasonic treatment on the ammonia-process powder caramel color at a certain ultrasonic frequency; and (4) controlling the ultrasonic power, the ultrasonic time and the ultrasonic temperature to obtain the ammonia-process powder caramel color after ultrasonic treatment. The Zeta potential of the caramel color subjected to ultrasonic treatment in a solution state is obviously increased, and when the Zeta potential is higher than 11.00 mV, the oxidation resistance of the treated ammonia-process powder caramel color is greatly improved, and meanwhile, the coloring power of the ammonia-process powder caramel color is also enhanced. The ammonia-process powder subjected to the ultrasonic treatment has a caramel color, and has better oxidation resistance and coloring ability.

Description

Technical Field

[0001] This invention belongs to the field of food additives, and specifically relates to a method for improving the antioxidant properties of caramel color from ammonia-processed powders. Background Technology

[0002] Caramel color is a brown or dark brown pigment formed by the dehydration, oxidation, and polymerization of sugars during heating. Its production process can be categorized into the ordinary method, the caustic sulfite method, the ammonia method, and the ammonium sulfite method. Among these, the ammonia method is the most widely used, found in the food industry for products such as soy sauce, vinegar, baking, candy, and beverages.

[0003] Caramel color is a type of large-molecule sugar polymer that contains antioxidant chemical components such as aldehydes, ketones, acids, alcohols, and unsaturated hydrocarbons, exhibiting a certain concentration-dependent antioxidant capacity. In recent years, much research and exploration has been conducted to improve the antioxidant capacity of caramel color, mainly focusing on chemical reactions or changes in the production process. Chinese invention patent CN113136113A utilizes low-temperature and high-temperature polymerization reactions to prepare conventional caramel color with improved antioxidant properties. Chinese invention patent CN114196228A obtains caramel color with good antioxidant capacity by crosslinking polyphenolic structures with sucrose molecules. Additionally, Chinese invention patent CN113397018A involves a primary reaction of raw starch syrup with an acid solution, followed by a secondary reaction with a Ti-Mg catalyst, generating a greater number of substituted furans, thereby significantly improving the antioxidant capacity of conventional caramel color. However, currently, there is no effective method to improve the antioxidant capacity of ammonia-processed caramel color.

[0004] As a non-thermal treatment technique, ultrasound offers advantages such as ease of implementation, low cost, and low energy consumption. It can influence the functional activity of biomolecules (polysaccharides, proteins, etc.) by altering their structure. Zeta potential is the net charge carried by a macromolecule in solution. Proteins or polysaccharides with high absolute Zeta potentials typically exhibit better activity, stemming from the presence of more charged active groups and better dispersibility and stability. Changing the Zeta potential of macromolecules through physical or chemical means can affect their activity.

[0005] Ammonia caramel color is the most widely used and produced type of caramel color. Improving the antioxidant properties of ammonia caramel color through ultrasound enhances its antioxidant effects in food products, thereby preventing oxidation and spoilage and extending their shelf life. Summary of the Invention

[0006] To address the above problems, this invention provides a method for improving the antioxidant properties of ammonia-processed caramel color powder. This method can enhance the antioxidant properties of ammonia-processed caramel color powder.

[0007] A method for improving the antioxidant properties of ammonia-processed caramel color powder includes the following steps:

[0008] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0009] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0010] (3) Under the protection of nitrogen, the ammonia-based caramel color powder is ultrasonically treated at a certain ultrasonic frequency;

[0011] (4) By controlling the ultrasonic power, ultrasonic time and ultrasonic temperature, the caramel color of the ammonia powder after ultrasonic treatment is obtained.

[0012] Furthermore, the ultrasonic frequency in step (3) is 40 kHz.

[0013] Furthermore, the ultrasonic power in step (4) is 200-350W.

[0014] Furthermore, the ultrasound time in step (4) is 1-20 min.

[0015] Furthermore, the ultrasonic temperature in step (4) is maintained at 20-45°C.

[0016] By placing ammonia-based caramel color powder in an ultrasonic environment, its antioxidant properties and coloring ability can be effectively improved, giving foods with added ammonia-based caramel color powder good antioxidant properties, thereby preventing or delaying the oxidative deterioration of the food and effectively extending its shelf life.

[0017] Compared with the prior art, the present invention has at least the following beneficial effects:

[0018] 1. This invention improves the zeta potential of ammonia-based caramel color powder in solution by using ultrasonic treatment.

[0019] 2. This invention improves the scavenging ability of ammonia-based caramel color powder and its iron ion reducing ability by ultrasonic treatment, thereby effectively enhancing its antioxidant properties.

[0020] 3. The caramel color solution obtained by this invention is bright red, which effectively improves its coloring ability and can achieve the desired coloring effect with the addition of a small amount of caramel color.

[0021] 4. The preparation process of this invention is simple and safe, with low cost and easy to industrialize. Attached Figure Description

[0022] Figure 1 The antioxidant capacity of the examples and comparative examples is shown (the horizontal axis represents the Zeta potential).

[0023] Figure 2 The antioxidant capacity and zeta potential of the examples and comparative examples are shown (the horizontal axis represents the sample name). Detailed Implementation

[0024] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the embodiments. The illustrative embodiments and descriptions of this invention are only used to explain this invention and are not intended to limit this invention.

[0025] Example 1:

[0026] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0027] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0028] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0029] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0030] (4) By controlling the ultrasonic power to 200W, the ultrasonic time to 5min and the ultrasonic temperature to 25-35℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0031] Example 2:

[0032] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0033] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0034] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0035] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0036] (4) By controlling the ultrasonic power to 250W, the ultrasonic time to 5min and the ultrasonic temperature to 25-35℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0037] Example 3:

[0038] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0039] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0040] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0041] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0042] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 5min and the ultrasonic temperature to 25-35℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0043] Example 4:

[0044] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0045] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0046] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0047] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0048] (4) By controlling the ultrasonic power to 350W, the ultrasonic time to 5min and the ultrasonic temperature to 25-35℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0049] Example 5:

[0050] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0051] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0052] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0053] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0054] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 5min and the ultrasonic temperature to 25-30℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0055] Example 6:

[0056] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0057] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0058] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0059] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0060] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 5min and the ultrasonic temperature to 30-35℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0061] Example 7:

[0062] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0063] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0064] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0065] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0066] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 5min and the ultrasonic temperature to 35-40℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0067] Example 8:

[0068] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0069] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0070] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0071] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0072] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 5min and the ultrasonic temperature to 40-45℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0073] Example 9:

[0074] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0075] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0076] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0077] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0078] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 1min and the ultrasonic temperature to 30℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0079] Example 10:

[0080] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0081] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0082] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0083] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0084] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 5min and the ultrasonic temperature to 30℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0085] Example 11:

[0086] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0087] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0088] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0089] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0090] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 10min and the ultrasonic temperature to 30℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0091] Example 12:

[0092] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0093] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0094] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0095] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0096] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 20min and the ultrasonic temperature to 30℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0097] Comparative Example 1:

[0098] This comparative example is based on Examples 1-12, and differs from Examples 1-12 in that:

[0099] The caramel color was not subjected to ultrasonic treatment. The physicochemical properties and antioxidant properties of the caramel colors prepared in Examples 1-12 and Comparative Example 1 were compared.

[0100] Comparative Example 2:

[0101] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0102] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0103] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0104] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0105] (4) By controlling the ultrasonic power to 300W, the ultrasonic time to 20min and the ultrasonic temperature to 55℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0106] Comparative Example 3:

[0107] This invention discloses a method for enhancing the antioxidant properties of ammonia-processed caramel color powder, which is prepared by the following steps:

[0108] (1) The ammonia-based caramel color powder is pretreated by ultra-fine grinding to 100-200 mesh;

[0109] (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas;

[0110] (3) Under the protection of nitrogen, the ammonia powder caramel color was ultrasonically treated at an ultrasonic frequency of 40 kHz.

[0111] (4) By controlling the ultrasonic power to 450W, the ultrasonic time to 25min and the ultrasonic temperature to 45℃, the ammonia powder caramel color after ultrasonic treatment was obtained.

[0112] Test samples: Caramel-colored samples prepared in Examples 1-12 and Comparative Examples 1-3.

[0113] Performance testing: The physicochemical properties and antioxidant properties of the caramel-colored samples prepared in Examples 1-12 and Comparative Examples 1-3 were tested respectively. The test methods are as follows:

[0114] 1. Physicochemical Indicators

[0115] (1) Absorbance test:

[0116] The test was conducted according to the method specified in GB 1886.64-2015, "Food Additives - Caramel Color". Weigh 0.25 g of the treated caramel color (accurate to 0.002 g), dissolve it in deionized water, transfer it to a 250 mL volumetric flask, dilute to the mark with deionized water, and shake well to obtain the sample solution. Place this sample solution in a 1 cm cuvette, using deionized water as a blank control, and measure its absorbance at 610 nm using a spectrophotometer. Absorbance indicates its coloring ability; the greater the absorption intensity, the stronger its coloring ability.

[0117] In addition to the 610nm light source required by the national food safety standard GB 1886.64-2015 "Food Additives - Caramel Color", the absorbance of caramel color also needs to be converted to obtain the color rate according to the industry-standard conversion method. The conversion formula is as follows:

[0118] (2) Color index (EBC units) measurement:

[0119]

[0120] (3) Zeta potential measurement

[0121] The zeta potential of treated and untreated caramel-colored samples was determined using a Malvern laser particle size analyzer to investigate the effects of factors such as ultrasonic treatment conditions on the zeta potential of caramel color.

[0122] The physicochemical properties of the caramel color prepared by this invention are shown in Table 1.

[0123] Table 1

[0124]

[0125]

[0126] 2. Antioxidant properties

[0127] (1) Determination of DPPH free radical scavenging ability

[0128] Weigh 0.05 g of the treated caramel color, dissolve it in deionized water, transfer it to a 500 mL volumetric flask, dilute to the mark with deionized water, and shake well to obtain the sample solution. Take 2 mL of the caramel color solution in a test tube, add 2 mL of 0.1 mmol / L DPPH ethanol solution, mix well, and react at room temperature in the dark for 30 min. Measure the absorbance at 517 nm. i The absorbance of a solution of 2 mL anhydrous ethanol and 2 mL caramel color was measured at 517 nm. The result was A. j The absorbance value (A0) was measured at 517 nm after mixing 2 mL of deionized water and 2 mL of DPPH ethanol solution and reacting at room temperature in the dark for 30 min. The DPPH free radical scavenging rate was calculated using the following formula:

[0129]

[0130] The antioxidant properties of the caramel color prepared in this invention are shown in Table 2.

[0131] (2) Determination of ABTS free radical scavenging ability

[0132] ABTS stock solution was prepared by mixing 7 mmol / L ABTS with 2.45 mmol / L potassium persulfate solution at a 1:1 (v:v) ratio and allowing it to stand at room temperature in the dark for 12 h. The ABTS stock solution was diluted with PBS solution (10 mmol / L, pH 7.4) until the absorbance at 734 nm was 0.70 ± 0.05 to prepare the ABTS working solution. 0.03 mL of caramel coloring solution (0.5 mg / mL) and 3 mL of ABTS working solution were mixed and allowed to stand at room temperature in the dark for 10 min. The absorbance was measured at 734 nm. a The absorbance value was measured using 3 mL of deionized water instead of the ABTS working solution. bThe absorbance value was measured using deionized water instead of the caramel-colored sample solution. c The ABTS radical scavenging rate is calculated using the following formula:

[0133]

[0134] (3) Determination of the reducing power of iron ions

[0135] Weigh 0.05 g of the above-treated caramel color, dissolve it in deionized water, transfer it to a 500 mL volumetric flask, dilute to the mark with deionized water, and shake well to obtain the sample solution. Then take 1 mL of the sample solution into a test tube, add phosphate buffer solution (0.2 mol / mL, pH 6.6) and 2.5 mL of 1% (w / v) potassium ferricyanide in sequence, mix well, heat in a water bath (50℃, 20 min), cool rapidly, add 2.5 mL of 10% (w / v) trichloroacetic acid, mix well, take out 2.5 mL, add 2.5 mL of deionized water and 0.5 mL of FeCl3 (0.1%, w / v), react fully for 20 min, and measure the absorbance at a wavelength of 700 nm.

[0136] Table 2

[0137]

[0138] As shown in Tables 1 and 2 above, in Examples 1-12 of this invention, by controlling the ultrasonic conditions to treat caramel color, the Zeta potential of ammonia-based caramel powder in solution can be increased. This is because ultrasonic treatment can change the dispersion degree of ammonia-based caramel powder, exposing some charged groups inside the macromolecular caramel color, thereby increasing its Zeta potential in solution, resulting in better dispersibility in solution, and thus reducing the steric hindrance for reaction with free radicals, thereby improving its antioxidant properties. Our experimental results show that within a certain range, increasing the ultrasonic power can improve the Zeta potential and antioxidant capacity of ammonia-based caramel powder; with increasing heating temperature or extending ultrasonic time, both the Zeta potential and antioxidant capacity decrease. However, when the Zeta potential > 11.00 mV, the antioxidant properties of caramel color are improved, and it also has good coloring ability. In contrast, the antioxidant properties of caramel color treated in Comparative Examples 2-3 decreased, indicating that ultrasound can improve the antioxidant properties of caramel color, but controlling the ultrasonic conditions is the key factor affecting the antioxidant properties of caramel color.

[0139] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for improving the antioxidant properties of caramel color in ammonia-processed powders, characterized in that, Includes the following steps: (1) Pre-treat the ammonia-based caramel color powder by ultra-fine grinding to 100-200 mesh; (2) Take the ammonia-based caramel color powder into the reaction vessel and introduce nitrogen gas; (3) Under the protection of nitrogen, the ammonia-based caramel color powder is ultrasonically treated at a certain ultrasonic frequency; (4) By controlling the ultrasonic power, ultrasonic time and ultrasonic temperature, the caramel color of the ammonia powder after ultrasonic treatment is obtained.

2. The method for improving the antioxidant properties of caramel color in ammonia-processed powders according to claim 1, characterized in that, The ultrasonic frequency in step (3) is 40 kHz.

3. The method for improving the antioxidant properties of ammonia-processed caramel color powder according to claim 1, characterized in that, The ultrasonic power in step (4) is 200-350W.

4. The method for improving the antioxidant properties of caramel color in ammonia-processed powders according to claim 1, characterized in that, The ultrasound time in step (4) is 1-20 min.

5. The method for improving the antioxidant properties of caramel color in ammonia-processed powders according to claim 1, characterized in that, The ultrasonic temperature in step (4) is maintained at 20-45℃.

6. The method for improving the antioxidant properties of ammonia-processed caramel color powder according to claim 1, characterized in that... The zeta potential of the caramel-colored ammonia powder after ultrasonic treatment is higher than 11.0 mV.

7. The method for improving the antioxidant properties of ammonia-processed caramel color powder according to claim 1, characterized in that... The ultrasonic treatment effectively improved the scavenging ability of DPPH and ABTS free radicals, as well as the iron ion reducing ability of the ammonia-based caramel powder.

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