Preparation method of high-temperature-resistant and photolysis-resistant composite pigment and application of composite pigment in meat products

Abstract

The invention relates to the technical field of preparation of composite pigments, in particular to a preparation method of a high-temperature-resistant photolysis-resistant composite pigment and application of the high-temperature-resistant photolysis-resistant composite pigment in meat products. According to the technical scheme, the method comprises the following steps: preparing the following raw materials in parts by weight: pigment base materials: 5-18 parts of monascus red pigment, 4-12 parts of high-color-value capsanthin and 3-8 parts of beta-cyclodextrin embedded curcumin; the component A comprises the following components in parts by weight: 1-5 parts of ascorbyl palmitate, 2-8 parts of polyglycerol fatty acid ester, 0.5-3 parts of L-sodium ascorbate and 0.1-1.5 parts of nano titanium dioxide; and 1 to 4 parts of N-acetyl-L-cysteine. The ultra-high stability of the natural pigment under the conditions of high-temperature processing and strong light irradiation is realized, the processing tolerance and the final color development effect are balanced, the problem of uneven dyeing caused by early release of the traditional pigment is solved, the product quality and the application convenience are improved, and the unification of safety and efficacy is realized.

Description

Technical Field

[0001] The present invention relates to the technical field of compound pigment preparation, and particularly to a preparation method of high-temperature resistant and photolysis-resistant compound pigment and its application in meat products. Background Art

[0002] With the continuous improvement of consumers' demand for the natural attributes of food, the application of natural pigments in meat products has become an industry development trend. However, the inherent thermal sensitivity and photo-instability of natural pigments severely restrict their wide application in modern food processing. This technical bottleneck is mainly reflected in the following aspects:

[0003] Insufficient thermal processing tolerance. Traditional natural pigments such as monascus red and capsanthin are prone to degradation reactions during high-temperature sterilization (121 - 135°C) and thermal processing of meat products, resulting in color attenuation and increased browning. Research shows that the retention rate of conventional monascus red pigment is less than 70% under the treatment of 121°C / 20min, and the degradation products may trigger the formation of off-flavor substances, directly affecting the product flavor.

[0004] The problem of photo-oxidation instability. The existing natural pigment system lacks an effective light protection mechanism and is prone to photolysis reactions under shelf-life light conditions (especially in the ultraviolet band). The ΔE value of commercially available curcumin pigments generally exceeds 3.0 after 12 hours of illumination at 4500 lux, resulting in deterioration of the product appearance and severely reducing consumer acceptance.

[0005] Limitations of stabilization technologies. The current mainstream solutions mostly rely on single chemical synthetic additives (such as BHT, TBHQ) or simple physical mixing processes, which have the following defects:

[0006] Chemical antioxidants may produce potential toxic by-products, which is contrary to the "clean label" trend;

[0007] Ordinary microencapsulation technology is difficult to balance the protection effect and processing release requirements, and often has too high a high-temperature capsule-breaking rate or insufficient terminal release;

[0008] Nanomaterials cause uneven dispersion due to agglomeration effects, which instead accelerates pigment oxidation;

[0009] Against this background, developing a compound pigment system that can simultaneously achieve high-temperature tolerance, photolysis inhibition, controlled release and meet food safety requirements has become the key technical direction to break through the application barrier of natural pigments. Therefore, this application proposes a preparation method of high-temperature resistant and photolysis-resistant compound pigment and its application in meat products. Summary of the Invention

[0010] The object of the present invention is to address the problem in the background art that there is no composite pigment system that can withstand high temperatures, inhibit photolysis, achieve controlled release, and meet food safety requirements, and to propose a preparation method for high-temperature resistant and photolysis-resistant composite pigments and their application in meat products.

[0011] In a first aspect, the present application provides a preparation method for high-temperature resistant and photolysis-resistant composite pigments, comprising the following steps:

[0012] S1. Prepare the following raw materials in parts by weight:

[0013] Pigment base material: 5 - 18 parts of monascus red pigment, 4 - 12 parts of high-color-value capsanthin, 3 - 8 parts of β-cyclodextrin-embedded curcumin;

[0014] Ascorbyl palmitate 1 - 5 parts, polyglycerol fatty acid ester 2 - 8 parts, sodium L-ascorbate 0.5 - 3 parts, nano-titanium dioxide 0.1 - 1.5 parts;

[0015] N-acetyl-L-cysteine 1 - 4 parts, epigallocatechin gallate (EGCG) 0.5 - 3 parts, sodium alginate 0.5 - 3 parts;

[0016] Propylene glycol 55 - 65 parts, deionized water 55 - 65 parts;

[0017] S2. Pre-emulsification stage: Mix propylene glycol and deionized water evenly, heat up to 45 - 55 °C, and sequentially add ascorbyl palmitate, polyglycerol fatty acid ester, and sodium L-ascorbate, and perform high-speed shear emulsification at 1000 - 1500 rpm for 10 - 15 minutes;

[0018] S3. Nano-dispersion: Add nano-titanium dioxide and use ultrasonic-microwave synergistic treatment for dispersion for 20 - 30 minutes;

[0019] S4. Gradient compounding: Add the pigment base material in three stages:

[0020] S401. First stage: Add monascus red pigment, maintain the temperature at 50 - 55 °C, and stir for 15 - 25 minutes;

[0021] S402. Second stage: Add high-color-value capsanthin, heat up to 60 - 65 °C, and mix at a rotation speed of 500 - 800 rpm;

[0022] S403. Third stage: Add β-cyclodextrin-embedded curcumin, cool down to 40 - 45 °C, and then stand for ripening for 1 - 2 hours;

[0023] S5. Stabilization treatment: Add the synergist component and perform microencapsulation through fluidized bed coating technology;

[0024] S6. Sterilization and packaging: Use high-voltage pulsed electric field treatment, and immediately perform aseptic filling after treatment.

[0025] Optionally, the β-cyclodextrin-embedded curcumin is prepared by the following process:

[0026] Mix curcumin and β-cyclodextrin in a molar ratio of 1:3 - 1:6, and add phosphate buffer solution with a pH of 6.5 - 7.2;

[0027] Adopt high-pressure microfluidization technology, circulate and process 3 - 5 times under a pressure of 150 - 200 MPa to form embedded particles with a particle size ≤ 200 nm.

[0028] Optionally, in the gradient composite stage, the oxygen content needs to be controlled ≤ 0.5%, and the viscosity change of the system needs to be detected at the interval of adding pigments in each stage. The next-stage feeding is carried out after the viscosity drops to 80% of the initial value.

[0029] Optionally, in S401, in the first stage: add monascus red pigment, maintain the temperature at 50 - 55 °C, and stir for 15 - 25 minutes under nitrogen protection.

[0030] Optionally, in S3, during the ultrasonic-microwave synergistic treatment, the ultrasonic power is 300 W, the microwave power is 200 W, and the frequency is 28 kHz.

[0031] Optionally, in S5, control the inlet air temperature at 60 - 70 °C, the atomization pressure at 0.15 - 0.25 MPa, and the coating weight gain rate at 10 - 15%.

[0032] Optionally, in S6, during the high-voltage pulsed electric field treatment, the field strength is 25 - 35 kV / cm, and the pulse width is 20 μs.

[0033] Optionally, in S1, prepare the following raw materials in parts by weight:

[0034] Pigment base material: 6 - 16 parts of monascus red pigment, 6 - 10 parts of high-color-value capsanthin, 4 - 7 parts of β-cyclodextrin-embedded curcumin;

[0035] 2 - 5 parts of ascorbyl palmitate, 3 - 7 parts of polyglycerol fatty acid ester, 1 - 3 parts of sodium L-ascorbate, 0.2 - 1.5 parts of nano-titanium dioxide;

[0036] 2 - 4 parts of N-acetyl-L-cysteine, 1 - 3 parts of epigallocatechin gallate (EGCG), 1 - 3 parts of sodium alginate;

[0037] 58 - 63 parts of propylene glycol, 58 - 63 parts of deionized water.

[0038] In the second aspect, the present application provides the application of the composite pigment prepared by the preparation method of the high-temperature resistant and light-decomposition resistant composite pigment described in the first aspect in meat products.

[0039] Compared with the prior art, the present application includes at least one of the following beneficial technical effects:

[0040] The ultra-high stability of natural pigments under high-temperature processing and strong light irradiation conditions is achieved, solving the technical problem of easy degradation of traditional natural pigments. The unique microcapsule structure design enables the pigment to remain stable during the processing and achieve efficient release in the end product, perfectly balancing the processing tolerance and the final color development effect.

[0041] The photothermal synergistic stabilization of β-cyclodextrin embedding and nano-titanium dioxide, and the three-dimensional protection network constructed by multiple antioxidants. Through the design of all-natural components and advanced processing techniques, not only the use of chemical synthetic additives is avoided, but it is also unexpectedly found that the embedding process can eliminate the potential toxicity of curcumin metabolites, achieving the unity of safety and efficacy.

[0042] Innovative processes such as high-voltage pulsed electric field treatment not only achieve efficient sterilization, but also produce additional effects such as the directional arrangement and self-permeability of pigment molecules, significantly improving the product quality and application convenience. It can be adapted to various meat product processing conditions, solving the industry pain point of limited application of traditional natural pigments in complex food systems, and providing new technical support for the development of clean label foods.

[0043] The present invention achieves the ultra-high stability of natural pigments under high-temperature processing and strong light irradiation conditions, balances the processing tolerance and the final color development effect, solves the problem of uneven staining caused by early release of traditional pigments, improves the product quality and application convenience, and realizes the unity of safety and efficacy. Detailed implementation manners

[0044] The technical solutions of the present invention will be further described below in conjunction with specific embodiments.

[0045] Example 1

[0046] The preparation method of the high-temperature resistant and photolysis-resistant composite pigment proposed in this example includes the following steps:

[0047] S1. Prepare the following raw materials in parts by weight:

[0048] Pigment base material: 5 parts of monascus pigment, 4 parts of high-color-value capsanthin, 3 parts of β-cyclodextrin-embedded curcumin; the β-cyclodextrin-embedded curcumin is prepared by the following process: mixing curcumin and β-cyclodextrin in a molar ratio of 1:3, adding a phosphate buffer solution with a pH of 6.5; using high-pressure microfluidization technology, circulating and treating 3 times at a pressure of 1500 MPa to form embedding particles with a particle size ≤ 200 nm;

[0049] 1 part of ascorbyl palmitate, 2 parts of polyglycerol fatty acid ester, 0.5 part of sodium L-ascorbate, 0.1 part of nano-titanium dioxide;

[0050] 1 part of N-acetyl-L-cysteine, 0.5 part of epigallocatechin gallate (EGCG), 0.5 part of sodium alginate;

[0051] 55 parts of propylene glycol, 55 parts of deionized water;

[0052] S2. Pre-emulsification stage: Mix propylene glycol and deionized water evenly, heat up to 45 °C, and sequentially add ascorbyl palmitate, polyglycerol fatty acid ester, and sodium L-ascorbate, and perform high-speed shear emulsification at 1000 rpm for 10 minutes;

[0053] S3. Nano-dispersion: Add nano-titanium dioxide, and use ultrasonic-microwave synergistic treatment to disperse for 20 minutes, with ultrasonic power of 300 W, microwave power of 200 W, and frequency of 28 kHz;

[0054] S4. Gradient compounding: Add pigment base materials in three stages: The oxygen content needs to be controlled ≤ 0.5% during the gradient compounding stage. The viscosity change of the system needs to be detected at the interval of adding pigments in each stage. When the viscosity drops to 80% of the initial value, then carry out the next stage of feeding;

[0055] S401. First stage: Add monascus red pigment, maintain the temperature at 50 °C, and stir for 15 - 25 minutes under nitrogen protection;

[0056] S402. Second stage: Add high-color-value capsanthin, heat up to 60 °C, and mix at a rotation speed of 500 rpm;

[0057] S403. Third stage: Add β-cyclodextrin-encapsulated curcumin, cool down to 40 °C, and then stand for ripening for 1 hour;

[0058] S5. Stabilization treatment: Add synergist components, and carry out microencapsulation through fluidized bed coating technology, control the inlet air temperature at 60 °C, atomization pressure at 0.15 MPa, and coating weight gain rate at 10%;

[0059] S6. Sterilization and filling: Use high-voltage pulsed electric field treatment, and immediately carry out aseptic filling after treatment. During the high-voltage pulsed electric field treatment, the field strength is 25 kV / cm, and the pulse width is 20 μs.

[0060] Example 2

[0061] The preparation method of the high-temperature resistant and light-photolysis resistant composite pigment proposed in this example is as follows:

[0062] S1. Prepare the following raw materials in parts by weight:

[0063] Pigment base materials: 8 parts of monascus red pigment, 7 parts of high-color-value capsanthin, 4 parts of β-cyclodextrin-embedded curcumin; the β-cyclodextrin-embedded curcumin is prepared by the following process: mixing curcumin and β-cyclodextrin at a molar ratio of 1:4, adding phosphate buffer solution with pH 6.7; adopting high-pressure microfluidization technology, circulating and treating 3 times at a pressure of 160 MPa to form embedding particles with a particle size ≤ 200 nm.

[0064] 2 parts of ascorbyl palmitate, 3 parts of polyglycerol fatty acid ester, 1 part of sodium L-ascorbate, 0.3 part of nano-titanium dioxide;

[0065] 2 parts of N-acetyl-L-cysteine, 1 part of epigallocatechin gallate (EGCG), 1 part of sodium alginate;

[0066] 58 parts of propylene glycol, 58 parts of deionized water;

[0067] S2. Pre-emulsification stage: Mix propylene glycol and deionized water evenly, heat up to 48 °C, and sequentially add ascorbyl palmitate, polyglycerol fatty acid ester, and sodium L-ascorbate, and perform high-speed shear emulsification at 1100 rpm for 11 minutes;

[0068] S3. Nano-dispersion: Add nano-titanium dioxide, and adopt ultrasonic-microwave synergistic treatment for dispersion for 22 minutes, with ultrasonic power of 300 W, microwave power of 200 W, and frequency of 28 kHz;

[0069] S4. Gradient compounding: Add pigment base materials in three stages: The oxygen content needs to be controlled ≤ 0.5% during the gradient compounding stage, and the viscosity change of the system needs to be detected at the addition interval of each stage of pigment. When the viscosity drops to 80% of the initial value, the next stage of feeding is carried out;

[0070] S401. First stage: Add monascus red pigment, maintain the temperature at 51 °C, and stir for 17 minutes under nitrogen protection;

[0071] S402. Second stage: Add high-color-value capsanthin, heat up to 61 °C, and mix at a rotation speed of 550 rpm;

[0072] S403. Third stage: Add β-cyclodextrin-embedded curcumin, cool down to 41 °C, and then stand and ripen for 1.2 hours;

[0073] S5. Stabilization treatment: Add synergist components, and carry out microencapsulation by fluidized bed coating technology, control the inlet air temperature at 62 °C, atomization pressure at 0.18 MPa, and coating weight gain rate at 11%;

[0074] S6. Sterilization and filling: Adopt high-voltage pulsed electric field treatment, and immediately carry out aseptic filling after treatment. During the high-voltage pulsed electric field treatment, the field strength is 28 kV / cm and the pulse width is 20 μs.

[0075] Example 3

[0076] The preparation method of the high-temperature resistant and photo-degradation resistant composite pigment proposed in this example comprises the following steps:

[0077] S1. Prepare the following raw materials by weight:

[0078] Pigment base material: 12 parts of monascus red pigment, 8 parts of high-color-value capsanthin, 6 parts of β-cyclodextrin-embedded curcumin; the β-cyclodextrin-embedded curcumin is prepared by the following process: mix curcumin and β-cyclodextrin at a molar ratio of 1:5, add phosphate buffer solution with pH 6.9; adopt high-pressure microfluidization technology, circulate and process 4 times under the pressure of 170 MPa to form embedded particles with a particle size ≤ 200 nm;

[0079] 3 parts of ascorbyl palmitate, 5 parts of polyglycerol fatty acid ester, 1.8 parts of sodium L-ascorbate, 0.8 part of nano-titanium dioxide;

[0080] 2.5 parts of N-acetyl-L-cysteine, 1.8 parts of epigallocatechin gallate (EGCG), 1.8 parts of sodium alginate;

[0081] 60 parts of propylene glycol, 60 parts of deionized water;

[0082] S2. Pre-emulsification stage: Mix propylene glycol and deionized water evenly, heat up to 50 °C, and sequentially add ascorbyl palmitate, polyglycerol fatty acid ester, and sodium L-ascorbate, and carry out high-speed shear emulsification at 1250 rpm for 12 minutes;

[0083] S3. Nano-dispersion: Add nano-titanium dioxide, and adopt ultrasonic-microwave synergistic treatment to disperse for 25 minutes, with ultrasonic power of 300 W, microwave power of 200 W, and frequency of 28 kHz;

[0084] S4. Gradient compounding: Add the pigment base material in three stages: the oxygen content needs to be controlled ≤ 0.5% during the gradient compounding stage, and the viscosity change of the system needs to be detected at the interval of adding pigments in each stage. When the viscosity drops to 80% of the initial value, then carry out the next stage of feeding;

[0085] S401. First stage: Add monascus red pigment, maintain the temperature at 53 °C, and stir for 20 minutes under nitrogen protection;

[0086] S402. Second stage: Add high-color-value capsanthin, heat up to 63 °C, and mix at a rotation speed of 650 rpm;

[0087] S403. Third stage: Add β-cyclodextrin-embedded curcumin, cool down to 43 °C, and then stand for ripening for 1.5 hours;

[0088] S5. Stabilization treatment: Add a synergist component, and perform microencapsulation through fluidized bed coating technology. Control the inlet air temperature at 65°C, the atomization pressure at 0.20 MPa, and the coating weight gain rate at 13%.

[0089] S6. Sterilization and filling: Use high-voltage pulsed electric field treatment, and immediately perform aseptic filling after treatment. During the high-voltage pulsed electric field treatment, the field strength is 30 kV / cm and the pulse width is 20 μs.

[0090] Example 4

[0091] The preparation method of the high-temperature resistant and photolysis-resistant composite pigment proposed in this example includes the following steps:

[0092] S1. Prepare the following raw materials in parts by weight:

[0093] Pigment base material: 16 parts of monascus red pigment, 10 parts of high-color-value capsanthin, 7 parts of β-cyclodextrin-embedded curcumin; the β-cyclodextrin-embedded curcumin is prepared by the following process: Mix curcumin and β-cyclodextrin in a molar ratio of 1:5, and add a phosphate buffer solution with a pH of 7.0; use high-pressure microfluidization technology to perform cyclic treatment 4 times at a pressure of 185 MPa to form embedded particles with a particle size ≤ 200 nm;

[0094] 4 parts of ascorbyl palmitate, 7 parts of polyglycerol fatty acid ester, 2.8 parts of L-ascorbate sodium, 1.2 parts of nano-titanium dioxide;

[0095] 3.5 parts of N-acetyl-L-cysteine, 2.8 parts of epigallocatechin gallate (EGCG), 2.8 parts of sodium alginate;

[0096] 62 parts of propylene glycol, 62 parts of deionized water;

[0097] S2. Pre-emulsification stage: Mix propylene glycol and deionized water evenly, heat up to 53°C, and sequentially add ascorbyl palmitate, polyglycerol fatty acid ester, and L-ascorbate sodium, and perform high-speed shear emulsification at 1400 rpm for 14 minutes;

[0098] S3. Nano-dispersion: Add nano-titanium dioxide, and use ultrasonic-microwave synergistic treatment to disperse for 28 minutes, with an ultrasonic power of 300 W, a microwave power of 200 W, and a frequency of 28 kHz;

[0099] S4. Gradient compounding: Add the pigment base material in three stages: During the gradient compounding stage, control the oxygen content ≤ 0.5%. The addition interval of pigments in each stage needs to detect the change in the system viscosity. When the viscosity drops to 80% of the initial value, then perform the next stage of feeding;

[0100] S401. The first stage: Add monascus red pigment, maintain the temperature at 54°C, and stir under nitrogen protection for 24 minutes;

[0101] S402, Second stage: Add high-color-value capsanthin, heat up to 64 °C, and mix at a rotation speed of 750 rpm;

[0102] S403, Third stage: Add β-cyclodextrin-encapsulated curcumin, cool down to 44 °C, and let it stand and ripen for 1.8 hours;

[0103] S5, Stabilization treatment: Add a synergist component, and perform microencapsulation through fluidized bed coating technology, controlling the inlet air temperature at 68 °C, the atomization pressure at 0.23 MPa, and the coating weight gain rate at 14%;

[0104] S6, Sterilization and filling: Use high-voltage pulsed electric field treatment, and immediately perform aseptic filling after treatment. During the high-voltage pulsed electric field treatment, the field strength is 32 kV / cm, and the pulse width is 20 μs.

[0105] Example 5

[0106] The preparation method of the high-temperature resistant and photolysis-resistant composite pigment proposed in this example includes the following steps:

[0107] S1, Prepare the following raw materials by weight:

[0108] Pigment base material: 18 parts of monascus red pigment, 12 parts of high-color-value capsanthin, 8 parts of β-cyclodextrin-encapsulated curcumin; The β-cyclodextrin-encapsulated curcumin is prepared by the following process: Mix curcumin and β-cyclodextrin in a molar ratio of 1:6, and add a phosphate buffer solution with a pH of 7.2; Use high-pressure microfluidization technology to circulate and process 5 times at a pressure of 200 MPa to form embedded particles with a particle size ≤ 200 nm;

[0109] 5 parts of ascorbyl palmitate, 8 parts of polyglycerol fatty acid ester, 3 parts of L-sodium ascorbate, 1.5 parts of nano-titanium dioxide;

[0110] 4 parts of N-acetyl-L-cysteine, 3 parts of epigallocatechin gallate (EGCG), 3 parts of sodium alginate;

[0111] 65 parts of propylene glycol, 65 parts of deionized water;

[0112] S2, Pre-emulsification stage: Mix propylene glycol and deionized water evenly, heat up to 55 °C, and sequentially add ascorbyl palmitate, polyglycerol fatty acid ester, and L-sodium ascorbate, and perform high-speed shear emulsification at 1500 rpm for 15 minutes;

[0113] S3, Nano-dispersion: Add nano-titanium dioxide, and use ultrasonic-microwave synergistic treatment to disperse for 30 minutes, with an ultrasonic power of 300 W, a microwave power of 200 W, and a frequency of 28 kHz;

[0114] S4. Gradient compounding: Add pigment base materials in three stages. During the gradient compounding stage, the oxygen content needs to be controlled at ≤0.5%. The viscosity change of the system needs to be detected at the interval of adding pigments in each stage. When the viscosity drops to 80% of the initial value, the next stage of feeding can be carried out.

[0115] S401. The first stage: Add monascus red pigment, maintain the temperature at 55°C, and stir for 25 minutes under nitrogen protection.

[0116] S402. The second stage: Add high-color-value capsanthin, heat up to 65°C, and mix at a speed of 800 rpm.

[0117] S403. The third stage: Add β-cyclodextrin-encapsulated curcumin, cool down to 40 - 45°C, and then stand for ripening for 1 - 2 hours.

[0118] S5. Stabilization treatment: Add a synergist component, carry out microencapsulation through fluidized bed coating technology, control the inlet air temperature at 70°C, the atomization pressure at 0.25 MPa, and the coating weight gain rate at 15%.

[0119] S6. Sterilization and filling: Use high-voltage pulsed electric field treatment, and immediately carry out aseptic filling after treatment. During the high-voltage pulsed electric field treatment, the field strength is 35 kV / cm and the pulse width is 20 μs.

[0120] Comparative example 1 (traditional pigment group):

[0121] Only use 18 parts of monascus red pigment

[0122] Carrier matrix: 65 parts of propylene glycol and 65 parts of deionized water

[0123] Preparation process: After conventional mixing, sterilize at 121°C for 15 minutes.

[0124] Comparative example 2 (lacking key component group):

[0125] Formula: The same as that of Example 5, but remove the β-cyclodextrin encapsulation process (directly use unencapsulated curcumin)

[0126] Process: Omit the fluidized bed microencapsulation step

[0127] Comparative example 3 (traditional process group):

[0128] Formula: The same as that of Example 5

[0129] Process:

[0130] Use a homogenizer to replace ultrasonic-microwave synergistic dispersion

[0131] Replace sterilization with heat sterilization at 121°C / 20 min.

[0132] Verify the pigment performance of the composite pigments in Examples 1-5 and the pigments in Comparative Examples 1-3, and conduct experiments;

[0133] 1. Comparative experiment: Difference in retention rate under the same processing conditions with traditional pigments (such as single monascus red) (design a heat treatment control group at 135°C / 30 min);

[0134] 2. Accelerated light exposure test: Verify the photodegradation resistance performance using the method of GB / T5009.35-2023.

[0135] Experimental methods and result analysis

[0136] 1. High-temperature resistance performance test (heat treatment at 135°C / 30 min)

[0137]

[0138] Conclusion:

[0139] The β-cyclodextrin embedding technology in Example 5 increased the retention rate of curcumin by 34.5% (Comparative Example 2); compared with traditional thermal sterilization (Comparative Example 3), the comprehensive retention rate of high-voltage pulsed electric field sterilization increased by 8.1%.

[0140] 2. Photodegradation resistance performance test (GB / T5009.35-2023)

[0141]

[0142] Key findings: The synergistic effect of nano-titanium dioxide and EGCG improved the light stability (ΔE in Example 5 decreased by 80.6% compared with Comparative Example 2); the microencapsulation structure effectively blocked the penetration of ultraviolet rays (TEM showed that the coating layer thickness reached 200-300 nm).

[0143] 3. Sustained-release performance test (simulating meat product processing)

[0144]

[0147] Mechanism verification: The porous structure (pore size 50-100 nm) formed by fluidized bed coating achieved physical barrier during the processing; sodium alginate underwent gelation transformation at high temperature, promoting controlled release in the final product.

[0148] Through the dual stability mechanism of molecular barrier construction and physical barrier coordination, the present invention achieves the thermal and light dual stability that is difficult to achieve in the traditional natural pigment system. The β-cyclodextrin embedding technology not only forms a steric hindrance effect at the molecular level, but its hydrophobic cavity more effectively isolates the thermosensitive groups of curcumin. Nano-titanium dioxide converts ultraviolet light into harmless heat energy through the surface plasmon resonance effect. The synergistic effect of the two produces a photothermal stability gain of 1 + 1 > 2. It is particularly noteworthy that during the high-temperature processing, the pigment components that are prone to the Maillard reaction originally show abnormal anti-browning characteristics, which stems from the redox buffer system constructed by EGCG and sodium L-ascorbate, and inhibits the non-enzymatic browning chain reaction by dynamically capturing free radicals. This effect far exceeds the theoretical protection limit of a single antioxidant.

[0149] The technical bottleneck of uneven dyeing caused by the early release of traditional pigments commonly existing in meat product processing is fundamentally solved by the intelligent release design in this solution. The porous microcapsule structure formed by fluidized bed coating maintains a dense state below 85 °C, effectively blocking the contact between the pigment and the processing medium; when the meat product reaches the cooking temperature, the synergistic phase change of sodium alginate and polyglycerol fatty acid ester realizes temperature-triggered controlled release. This precise release behavior not only avoids processing losses, but also improves the color uniformity of the final product to a level indistinguishable to the naked eye, and its process adaptability breaks through the inherent understanding of the application scenarios of natural pigments in the existing technology.

[0150] Embedding-dispersion synergy: The β-cyclodextrin embedding of curcumin and the nano-titanium dioxide dispersion system produce a unique photothermal response synergy. The embedding structure absorbs near-infrared heat to promote the electron transition on the surface of the nanoparticles, which instead enhances the reflection efficiency in the visible light band. This phenomenon has not been reported in the existing literature, showing an energy transfer type synergy gain between components.

[0151] Antioxidant network effect: The sulfhydryl group of N-acetylcysteine and the phenolic hydroxyl group of EGCG form a dynamic redox pair, and a three-dimensional free radical scavenging network is constructed under the mediation of ascorbyl palmitate. Its antioxidant efficiency shows an exponential increase compared with single components, and it even maintains continuous activity after multiple thermal shocks, showing excellent antioxidant durability.

[0152] Process-component coupling and synergistic enhancement: The temperature-shear force control in stages in the gradient composite process enables the formation of an ordered arrangement structure of each pigment molecule. The preferential dispersion of monascus red pigment at the low temperature stage forms a three-dimensional scaffold, and the embedding of capsanthin at the medium temperature stage enhances the π-π stacking interaction between molecules. Finally, the introduction of curcumin at low temperature fills the lattice defects. This molecular-level spatial assembly makes a qualitative leap in the stability of the system.

[0153] Traditional pigment stabilization techniques often rely on synthetic additives, while this solution achieves the unity of safety and efficacy through the functional recombination of natural components. It is particularly noteworthy that: while the β-cyclodextrin inclusion process improves the bioavailability of curcumin, trace cytotoxic substances originally present in its metabolites are completely eliminated, and toxicological verification shows an improved toxicological property effect. In addition, through surface modification technology, the dissolution rate of nano-titanium dioxide in an acidic digestion environment is less than 0.1%, fundamentally solving the migration risk of nanomaterials.

[0154] The introduction of high-pressure pulsed electric field sterilization technology not only avoids the degradation of heat-sensitive components, but also unexpectedly discovers its electric field-induced orientation effect: pulsed treatment causes pigment molecules to be oriented, significantly enhancing the color development intensity (the color value increases by 15 - 20% under the same dosage). The ultrasonic-microwave synergistic dispersion not only achieves the monodispersion of nanoparticles, but also induces a stable gas-liquid interface in the carrier matrix, enabling the final product to have self-permeation characteristics during meat product injection processing, significantly improving the dyeing efficiency and uniformity.

[0155] This invention breakthroughly integrates molecular inclusion, nanotechnology, and physical field regulation across disciplines, realizes the zero-loss application of natural pigments under extreme processing conditions, and solves the problem of color fading caused by high-temperature sterilization of meat products. It establishes an environmentally responsive release mechanism, upgrading the pigment function from simple coloring to a processing indicator. It creates a self-protective antioxidant system that remains continuously stable in an open processing environment. Through the cascading transfer of energy levels between components, photodegradation by-products are converted into a stabilization driving force.

[0156] Through a dual stabilization mechanism that combines molecular barriers and physical barriers, such as the photothermal synergistic stabilization of β-cyclodextrin inclusion and nano-titanium dioxide, and the three-dimensional protection network constructed by multiple antioxidants, the ultra-high stability of natural pigments under high-temperature processing and strong light irradiation conditions is achieved, solving the technical problem of easy degradation of traditional natural pigments; the unique fluidized bed coating microcapsule structure design forms temperature-triggered controlled release, balancing processing tolerance and final color development effect, and solving the problem of uneven dyeing caused by early release of traditional pigments; innovative processes such as ultrasonic-microwave synergistic treatment and high-pressure pulsed electric field treatment produce additional effects such as the oriented arrangement and self-permeability of pigment molecules, improving product quality and application convenience; the all-natural component design avoids the use of chemical synthetic additives, the inclusion process eliminates the potential toxicity of curcumin metabolites, and the surface modification of nano-titanium dioxide reduces the migration risk, achieving the unity of safety and efficacy; the gradient composite process enables each pigment molecule to form an ordered arrangement structure, enhancing the system stability. This invention breaks through the traditional technical bottleneck, provides new support for the development of clean label foods, and demonstrates significant technological breakthroughs and industrial application value.

[0157] The above specific embodiments are merely several alternative embodiments of the present invention. Based on the technical solution of the present invention and the relevant revelations of the above embodiments, those skilled in the art can make various alternative improvements and combinations to the above specific embodiments.

Claims

1. A method for preparing a high temperature resistant and photolysis resistant composite pigment, characterized in that: The following steps are involved: S1, prepare the following raw materials by weight: Pigment base: 5-18 parts of monascus red pigment, 4-12 parts of high color value capsanthin, 3-8 parts of β-cyclodextrin-encapsulated curcumin; 1-5 parts of ascorbyl palmitate, 2-8 parts of polyglycerol fatty acid ester, 0.5-3 parts of L-sodium ascorbate, 0.1-1.5 parts of nano titanium dioxide; 1-4 parts of N-acetyl-L-cysteine, 0.5-3 parts of epigallocatechin gallate, and 0.5-3 parts of sodium alginate; 55-65 parts of propylene glycol, 55-65 parts of deionized water; S2, pre-emulsification stage: propylene glycol and deionized water are mixed evenly, the temperature is raised to 45-55°C, ascorbyl palmitate, polyglycerol fatty acid ester, and sodium L-ascorbate are added in sequence, and emulsification is performed at a high shear speed of 1000-1500 rpm for 10-15 minutes; S3, nano-dispersion: adding nano-titanium dioxide and dispersing it by ultrasonic-microwave synergistic treatment for 20-30 minutes; S4, Gradient compounding: Add pigment base in three stages: S401, first stage: add red pigment of Monascus, maintain the temperature at 50-55°C, and stir for 15-25 minutes; S402, second stage: adding high color value capsanthin, heating to 60-65°C, and mixing at 500-800 rpm; S403, the third stage: adding β-cyclodextrin to encapsulate curcumin, cooling to 40-45°C and then standing for 1-2 hours; S5, stabilization treatment: adding synergist components and microencapsulating by fluidized bed coating technology; S6. Sterilization and packaging: Use high-voltage pulse electric field treatment and sterile filling immediately after treatment.

2. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: The β-cyclodextrin-embedded curcumin is prepared by the following process: Curcumin and β-cyclodextrin were mixed in a molar ratio of 1:3-1:6, and a phosphate buffer solution of pH 6.5-7.2 was added; Using high-pressure microfluidics technology, the process is cyclically treated 3-5 times at a pressure of 150-200MPa to form embedded particles with a particle size of ≤200nm.

3. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: The oxygen content in the gradient compound stage needs to be controlled to be ≤0.5%, and the viscosity change of the system needs to be detected at the interval of adding pigments in each stage. When the viscosity drops to 80% of the initial value, the next stage of feeding can be carried out.

4. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: In the S401, the first stage: add Monascus red pigment, maintain the temperature at 50-55° C., and stir for 15-25 minutes under nitrogen protection.

5. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: In S3, during the ultrasound-microwave synergistic treatment, the ultrasound power is 300 W, the microwave power is 200 W, and the frequency is 28 kHz.

6. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: In S5, the air inlet temperature is controlled at 60-70° C., the atomization pressure is controlled at 0.15-0.25 MPa, and the coating weight gain rate is controlled at 10-15%.

7. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: In the S6, during the high voltage pulse electric field treatment, the field strength is 25-35 kV / cm and the pulse width is 20 μs.

8. The method for preparing the high temperature resistant and photolysis resistant composite pigment according to claim 1, characterized in that: In S1, the following raw materials in parts by weight are prepared: Pigment base: 6-16 parts of monascus red pigment, 6-10 parts of high color value capsanthin, 4-7 parts of β-cyclodextrin-encapsulated curcumin; 2-5 parts of ascorbyl palmitate, 3-7 parts of polyglycerol fatty acid ester, 1-3 parts of L-sodium ascorbate, 0.2-1.5 parts of nano titanium dioxide; 2-4 parts of N-acetyl-L-cysteine, 1-3 parts of epigallocatechin gallate (EGCG), and 1-3 parts of sodium alginate; 58-63 parts of propylene glycol and 58-63 parts of deionized water.

9. Use of the composite pigment prepared by the method for preparing the high temperature resistant and photolysis resistant composite pigment according to any one of claims 1 to 8 in meat products.

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