Pericarpium citri reticulatae pigment, preparation method thereof and blasting bead wall material

Abstract

The invention provides a preparation process of a pericarpium citri reticulatae pigment, which comprises the following steps: A) crushing pericarpium citri reticulatae to obtain pericarpium citri reticulatae powder; adding the dried orange peel powder into the fermentation culture medium, and fermenting to obtain a fermented mixture; b) performing ultrasonic extraction, centrifugation or filtration on the fermented mixture to obtain an extracting solution containing the pericarpium citri reticulatae pigment; and C) concentrating the extracting solution containing the pericarpium citri reticulatae pigment, purifying with resin, and freeze-drying to obtain the pericarpium citri reticulatae pigment. The pericarpium citri reticulatae pigment is prepared by taking pericarpium citri reticulatae as a raw material and combining ultrasonic assistance with a fermentation treatment method, the process is simple, the damage of high temperature to the pigment can be avoided, the effective release of the pigment is promoted, and the prepared pericarpium citri reticulatae pigment is high in stability and high in extraction rate. According to the method, the tangerine peel pigment is purified by adopting a macroporous resin method, so that impurities including soluble protein, fiber, sugar and the like contained in the pigment crude extract can be effectively removed, the quality of the tangerine peel pigment product is improved, and the application range is wider.

Description

Technical Field

[0001] The invention relates to the technical field of tobacco, in particular to a tangerine peel pigment and a preparation method thereof and a popping bead wall material. Background Art

[0002] Tangerine peel (Pericarpium Citri Reticulatae, PCR) is the dried mature peel cultivated for the genus Citrus and its variants of the Rutaceae family. It has a strong taste and is slightly bitter. It has medicinal effects such as relieving cough and reducing phlegm, regulating the spleen and lungs, and regulating qi. It is a very good traditional Chinese medicine. In addition, it is also a spice and condiment. Tangerine peel is rich in a variety of bioactive substances, including flavonoids, carotenoids, alkaloids, essential oils, phenolic acids, terpenoid compounds, etc., and has antioxidant, anti-tumor, pain relief, and anti-neuroinflammatory effects.

[0003] Edible pigments are the main components of food additives. They are not only widely used in the food industry to improve the color of food and increase people's enjoyment of beauty, but also widely used in tobacco industry cigarette popping beads to increase the external quality of popping beads. Among them, natural pigments are not only non-toxic and harmless, environmentally friendly, but also have the color and unique aroma of the food itself. Tangerine peel pigment components have multiple physiological activities such as antioxidant and anti-inflammatory. However, the existing tangerine peel pigment extraction methods have problems such as low extraction efficiency, low product purity, and poor stability, which limits its application in the field of popping beads.

[0004] Therefore, it is of great practical significance to develop an efficient, environmentally friendly and highly stable method for extracting and preparing tangerine peel pigment and its application in popping bead wall materials. Summary of the invention

[0005] In view of this, the technical problem to be solved by the present invention is to provide a method for preparing tangerine peel pigment. The tangerine peel pigment provided by the present invention has strong stability, high extraction rate, and good sensory perception. At the same time, the prepared blasting bead wall material has uniform color and good stability.

[0006] The present invention provides a preparation process of tangerine peel pigment, comprising the following steps:

[0007] A) crushing tangerine peel to obtain tangerine peel powder; adding the tangerine peel powder to a fermentation medium, fermenting, and obtaining a fermented mixture;

[0008] B) ultrasonically extracting the fermented mixture, centrifuging or filtering to obtain an extract containing orange peel pigment;

[0009] C) The extract containing tangerine peel pigment is concentrated, purified by resin, and freeze-dried to obtain the product.

[0010] Preferably, in step A), the pulverizing is performed by passing through a 60-80 mesh sieve.

[0011] Preferably, in step A), the microbial strains in the fermentation medium include Aspergillus oryzae and / or yeast, and the strain concentration is 5-30%;

[0012] The solid-liquid ratio of the tangerine peel powder to the culture medium is 1:8-1:24; the fermentation temperature is 20-45°C, and the fermentation time is 12-48 hours; the initial pH value of the fermentation is adjusted to 5.0-9.0 using a buffer solution; the buffer solution can be a phosphate solution, a Tris buffer solution or a citric acid-sodium citrate solution.

[0013] Preferably, in step B), the solvent for the ultrasonic extraction includes ethanol, acetone or ethyl acetate; the solid-liquid ratio of the ultrasonic extraction is 1:4-1:30; the temperature of the ultrasonic extraction is 30-60°C, and the time is 20-60 min.

[0014] Preferably, the centrifugal parameters in step B) include 4000-8000 r / min, centrifugation for 5-15 min;

[0015] The filter membrane used in the filtration is a nanofiltration membrane; the pore size of the filter membrane is 0.8-1 μm.

[0016] Preferably, the concentration in step C) is rotary evaporation concentration, and the parameters of the rotary evaporation include 0.1-0.55Mpa, 40-65°C;

[0017] The resin includes X-5, BM-2, AB-8 or D101; the pretreatment of the resin is as follows: soaking the resin in 95% ethanol for 24 to 48 hours to fully swell, rinsing with 95% ethanol, washing the ethanol with distilled water, soaking and rinsing with 1% to 5% HCL solution, washing with distilled water until neutral, then soaking and rinsing with 1% to 5% NaOH solution, and finally washing with distilled water until neutral for standby use;

[0018] The static adsorption and desorption conditions of the resin are as follows: the pH of the extract containing tangerine peel pigment is 6.0~9.0, the ethanol elution concentration is 40%~70%, the sample volume is 200~350mL, and the eluent volume is 100~250mL.

[0019] Preferably, the freeze-drying parameters in step C) include:

[0020] Pre-freezing: Pre-freeze the orange peel pigment at -18 to -20°C for 24 to 48 hours;

[0021] Sublimation drying: sublimation drying at -20 to -45°C for 12 to 24 hours, vacuum degree 45 to 80 Pa;

[0022] Desorption drying: Desorption drying at 20-45°C for 4-6 hours, vacuum degree 10-50Pa.

[0023] The invention provides a tangerine peel pigment, which is prepared by the preparation method described in any one of the above technical solutions.

[0024] The present invention provides a bead-blasting wall material, comprising the following raw materials in parts by weight:

[0025] 3-6 parts of sodium alginate, 4-8 parts of agar, 2-4 parts of glycerin, 0.02-0.04 parts of tangerine peel pigment, 0.002-0.004 parts of VC, VE or citric acid, and 80-100 parts of solvent;

[0026] The solvent is 0.1% to 0.5% acetic acid water or 0.01% to 0.2% lactic acid water.

[0027] The present invention provides a bursting bead, comprising the bursting bead wall material described in the above technical solution.

[0028] Compared with the prior art, the present invention provides a preparation process of tangerine peel pigment, comprising the following steps: A) crushing tangerine peel to obtain tangerine peel powder; adding tangerine peel powder to a fermentation medium, fermenting, and obtaining a fermented mixture; B) ultrasonically extracting the fermented mixture, centrifuging or filtering, and obtaining an extract containing tangerine peel pigment; C) concentrating the extract containing tangerine peel pigment, resin purification, and freeze-drying. The present invention uses tangerine peel as a raw material, and adopts an ultrasound-assisted combined fermentation treatment method to prepare tangerine peel pigment. The process is simple, can avoid the damage of high temperature to the pigment, promote the effective release of the pigment, and the prepared tangerine peel pigment has strong stability and high extraction rate. The present invention adopts a macroporous resin method to purify tangerine peel pigment, which can effectively remove impurities contained in the crude pigment extract, including soluble protein, fiber and sugar, etc., so that the quality of tangerine peel pigment products is improved and the scope of application is wider. DETAILED DESCRIPTION

[0029] The present invention provides a tangerine peel pigment and a preparation method thereof and a blasting bead wall material. Those skilled in the art can refer to the content of this article and appropriately improve the process parameters to achieve it. It should be particularly pointed out that all similar replacements and modifications are obvious to those skilled in the art, and they all belong to the scope of protection of the present invention. The method and application of the present invention have been described through preferred embodiments, and relevant personnel can obviously modify or appropriately change and combine the method and application of this article without departing from the content, spirit and scope of the present invention to realize and apply the technology of the present invention.

[0030] In this application, the term "and / or" describes the association relationship of associated objects, indicating that there may be three relationships. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. A and B can be singular or plural.

[0031] The tangerine peel pigment described in the present invention refers to a general term for various natural pigments that impart color to tangerine peel.

[0032] The present invention provides a preparation process of tangerine peel pigment, comprising the following steps:

[0033] A) crushing tangerine peel to obtain tangerine peel powder; adding the tangerine peel powder to a fermentation medium, fermenting, and obtaining a fermented mixture;

[0034] B) ultrasonically extracting the fermented mixture, centrifuging or filtering to obtain an extract containing orange peel pigment;

[0035] C) The extract containing tangerine peel pigment is concentrated, purified by resin, and freeze-dried to obtain the product.

[0036] The preparation process of tangerine peel pigment provided by the present invention comprises the following steps: firstly, pre-treating raw materials, selecting undamaged and high-quality tangerine peel raw materials, ensuring that the tangerine peel raw materials are fresh, dry and free from mildew, crushing the tangerine peel with a pulverizer, and passing through a sieve to obtain tangerine peel powder; the crushing step is passing through a 60-80 mesh sieve after the crushing step.

[0037] The tangerine peel powder is added into a fermentation medium and fermented to obtain a fermented mixture.

[0038] Take tangerine peel powder, add it to fermentation medium, add cultured microbial culture liquid, adjust to a suitable pH value with a buffer at a suitable temperature, ferment for a certain period of time, and promote the release of pigments.

[0039] The microbial strains in the fermentation medium of the present invention include Aspergillus oryzae and / or yeast, and the strain concentration is 5-30%;

[0040] The solid-liquid ratio of the tangerine peel powder to the culture medium is 1:8-1:24; specifically, it can be 1:8, 1:10, 1:14, 1:16, 1:18, 1:20, 1:24; or a range value between any two of the above.

[0041] The fermentation temperature is 20-45°C, specifically 20°C, 25°C, 30°C, 35°C, 40°C, 45°C; or a range between any two of the above.

[0042] The fermentation time is 12 to 48 hours; specifically, it can be 12 hours, 20 hours, 24 hours, 40 hours or 48 hours; or a range between any two of the above.

[0043] The initial pH value of the fermentation is adjusted to 5.0-9.0 using a buffer solution, and specifically can be 5.0, 6.0, 7.0, 8.0 or 9.0, or a range between any two of the above.

[0044] The buffer may be phosphate solution, Tris buffer or citric acid-sodium citrate.

[0045] The fermented mixture is extracted by ultrasonic. By adjusting the material-liquid ratio, ultrasonic time, and ultrasonic temperature, the mechanical and thermal effects of ultrasound are used to further accelerate the fermentation reaction, while destroying the cell wall and releasing more pigments.

[0046] The solvent for ultrasonic extraction of the present invention includes ethanol, acetone or ethyl acetate; the material-liquid ratio of the ultrasonic extraction is 1:4-1:30; 1:4, 1:5, 1:8, 1:10, 1:14, 1:16, 1:18, 1:20, 1:24, 1:30; or a range value between any two of the above.

[0047] The temperature of ultrasonic extraction is 30-60°C, specifically 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C; or a range between any two of the above.

[0048] The ultrasonic extraction time is 20 to 60 minutes, preferably 20 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes, or a range between any two of the above.

[0049] After the ultrasonic treatment, the mixture is centrifuged or filtered through a membrane to remove unreacted raw material residues and bacterial solution, and the supernatant is collected, i.e., the extract containing tangerine peel pigment.

[0050] The centrifugal parameters of the present invention include 4000-8000 r / min, specifically 4000 r / min, 5000 r / min, 6000 r / min, 7000 r / min, 8000 r / min; or a range value between any two of the above.

[0051] The centrifugation time is 5 to 15 minutes, specifically 5 minutes, 10 minutes or 15 minutes, or a range between any two of the above.

[0052] The filter membrane used in the filtration of the present invention is a nanofiltration membrane; the pore size of the filter membrane is 0.8-1 μm, which can be 0.8 μm, 0.9 μm or 1 μm, or a range between any two of the above.

[0053] The extract is concentrated and the solvent is recovered to obtain a crude extract of tangerine peel pigment. The concentration is rotary evaporation concentration, and the rotary evaporation pressure is 0.1-0.55 MPa, specifically 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa, 0.5 MPa, 0.55 MPa, or any range between the above two values.

[0054] The temperature of the rotary evaporation is 40-65°C; 40°C, 45°C, 50°C, 55°C, 65°C; or a range between any two of the above.

[0055] The crude extract of tangerine peel pigment is separated and purified by using pretreated macroporous resin to obtain a high-purity pigment product.

[0056] The resin of the present invention includes X-5, BM-2, AB-8 or D101;

[0057] The pretreatment of the resin is as follows: soak the resin in 95% ethanol for 24-48 hours to fully swell, rinse with 95% ethanol, wash the ethanol with distilled water, soak and rinse with 1%-5% HCL solution, then wash with distilled water until neutral, then soak and rinse with 1%-5% NaOH solution, finally wash with distilled water until neutral, and set aside;

[0058] The static adsorption and desorption conditions of the resin are as follows: the pH of the extract containing tangerine peel pigment is 6.0~9.0, the ethanol elution concentration is 40%~70%, the sample volume is 200~350mL, and the eluent volume is 100~250mL.

[0059] The purified tangerine peel pigment extract is freeze-dried to collect tangerine peel pigment powder.

[0060] The freeze-drying parameters of the present invention include:

[0061] Pre-freezing: Pre-freeze the orange peel pigment at -18 to -20°C for 24 to 48 hours;

[0062] Sublimation drying: sublimation drying at -20 to -45°C for 12 to 24 hours, vacuum degree 45 to 80 Pa;

[0063] Desorption drying: Desorption drying at 20-45°C for 4-6 hours, vacuum degree 10-50Pa.

[0064] The process of the invention can significantly improve the extraction rate of tangerine peel pigment, retain the tangerine peel pigment components to the greatest extent, and separate and purify the pigment by a macroporous resin method, which can significantly improve the purity of tangerine peel pigment. Compared with the traditional extraction process, the tangerine peel pigment prepared by the process has a high extraction rate, good product quality and strong stability.

[0065] The invention provides a tangerine peel pigment, which is prepared by the preparation method described in any one of the above technical solutions.

[0066] The present invention has clearly described the above specific preparation method, which will not be repeated here.

[0067] The present invention provides a bead-blasting wall material, comprising the following raw materials in parts by weight:

[0068] 3-6 parts of sodium alginate, 4-8 parts of agar, 2-4 parts of glycerin, 0.02-0.04 parts of tangerine peel pigment, 0.002-0.004 parts of VC, VE or citric acid, and 80-100 parts of solvent;

[0069] The solvent is 0.1% to 0.5% acetic acid water or 0.01% to 0.2% lactic acid water.

[0070] In some preferred embodiments, the blasting bead wall material comprises the following raw materials in parts by weight: 4 parts of sodium alginate, 6 parts of agar, 3 parts of glycerol, 0.03 parts of tangerine peel pigment, 0.003 parts of VC, and the solvent is 100 parts of 0.2% acetic acid water.

[0071] In some preferred embodiments, the blasting bead wall material comprises the following raw materials in parts by weight:

[0072] 3 parts of sodium alginate, 4 parts of agar, 2 parts of glycerin, 0.02 parts of tangerine peel pigment, 0.002 parts of VE, and the solvent is 80 parts of 0.5% acetic acid water.

[0073] The tangerine peel pigment prepared by the invention is applied to the popping bead wall material, and the prepared popping bead wall material has the peculiar color and aroma of tangerine peel and has strong antioxidant activity.

[0074] The invention adopts ultrasound-assisted combined fermentation method to prepare tangerine peel pigment, purifies tangerine peel pigment by macroporous resin method, and applies it to the process of popping pearl wall material. The extraction method of the invention has simple process, pigment substances are not easy to be destroyed, and the extraction rate is high. At the same time, the prepared popping pearl wall material has stable color and rich tangerine peel aroma.

[0075] The present invention provides a bursting bead, comprising the bursting bead wall material described in the above technical solution.

[0076] The present invention provides a formula for popping bead wall materials for cigarettes. Since tangerine peel pigment has good antioxidant and anti-inflammatory effects, compared with the traditional popping bead wall material formula, the amount of additives used is reduced. At the same time, the prepared popping beads have the unique aroma of tangerine peel and add visual appeal to the popping beads. The present invention uses natural tangerine peel pigment instead of synthetic pigment in the popping bead wall material formula, which can effectively reduce the impact on the environment during the production process, conforming to the concept of sustainable development, and natural pigments are safer than synthetic pigments and more in line with the edible characteristics of popping beads. Tangerine peel pigment is used in the popping bead wall material, processed by microencapsulation and other technologies, and antioxidants are added to the formula, which improves the stability of the tangerine peel pigment and helps to maintain the color stability of the popping beads.

[0077] The present invention provides a preparation process of tangerine peel pigment, comprising the following steps: A) crushing tangerine peel to obtain tangerine peel powder; adding tangerine peel powder to fermentation medium, fermenting, and obtaining a fermented mixture; B) ultrasonically extracting the fermented mixture, centrifuging or filtering, and obtaining an extract containing tangerine peel pigment; C) concentrating the extract containing tangerine peel pigment, resin purification, and freeze-drying. The present invention uses tangerine peel as a raw material, and adopts an ultrasound-assisted combined fermentation treatment method to prepare tangerine peel pigment. The process is simple, can avoid the damage of high temperature to the pigment, promote the effective release of the pigment, and the prepared tangerine peel pigment has strong stability and high extraction rate. The present invention adopts a macroporous resin method to purify tangerine peel pigment, which can effectively remove impurities contained in the crude pigment extract, including soluble protein, fiber and sugar, so that the quality of tangerine peel pigment products is improved and the scope of application is wider.

[0078] It should be understood that in the various embodiments of the present application, the size of the serial numbers of the above-mentioned processes does not mean the order of execution, some or all of the steps can be executed in parallel or sequentially, and the execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.

[0079] The numerical ranges and parameters involved in the present invention have presented the relevant numerical values ​​in the specific embodiments as accurately as possible. However, any numerical value essentially inevitably contains standard deviations due to individual testing methods. Therefore, unless otherwise explicitly stated, it should be understood that all numerical ranges or specific data used in this disclosure may have certain reasonable deviations within a certain range, for example: within 1% or 0.5%.

[0080] Some cases are recorded in the embodiments and comparative examples of the present invention, wherein the embodiments show certain implementation modes of the present invention. However, this does not mean that the effects of the present invention can only be achieved in these cases.

[0081] In order to further illustrate the present invention, a tangerine peel pigment, a preparation method thereof and a blasting bead wall material provided by the present invention are described in detail below in conjunction with embodiments.

[0082] Embodiment 1:

[0083] (1) Select intact, high-quality tangerine peel raw materials, ensuring that they are fresh, dry and free of mold;

[0084] (2) taking the dried tangerine peel raw material of step (1), crushing it with a crusher, and passing it through a 60-mesh sieve to obtain dried tangerine peel powder;

[0085] (3) Weigh 50 g of tangerine peel powder, add 500 g of culture medium, inoculate 10% Aspergillus oryzae + 10% yeast strain, and ferment at 40°C and pH 8.0 for 24 h to promote the release of pigment.

[0086] (4) The fermented mixture was placed in an ultrasonic extractor with acetone as the extraction solvent. The volume ratio of the fermentation mixture to acetone was 1:10. Ultrasonic extraction was performed at 40°C for 30 min. The mechanical and thermal effects of ultrasound were used to further accelerate the fermentation reaction, while destroying the cell wall and releasing more pigments.

[0087] (5) After the ultrasonic treatment, the mixture was centrifuged at 6000 r / min for 10 min, and the supernatant was filtered through a 0.8 um filter membrane to remove the unreacted raw material residue and bacterial solution, i.e., the extract containing tangerine peel pigment.

[0088] (6) The extract was concentrated by rotary evaporation at 0.1 MPa and 45°C to 20% of the original volume to prepare tangerine peel pigment extract with a yield of 20.5%.

[0089] (7) The crude extract of tangerine peel pigment in step (6) was purified by separation using X-5 macroporous resin after pretreatment, with the pH of the tangerine peel pigment solution adjusted to 6.0, the ethanol elution concentration being 40%, the sample volume being 250 mL, and the eluent volume being 200 mL to obtain a high-purity pigment product. The purity of the tangerine peel pigment reached 80.2%.

[0090] (8) The purified tangerine peel pigment was freeze-dried in a freeze dryer at -18°C for 24 h. The sublimation and analytical drying temperatures were -20°C and 35°C, respectively, and the vacuum degrees were 45 Pa and 30 Pa, respectively. The tangerine peel pigment powder was collected and the pigment content was measured to be 10.7 g / 100 g.

[0091] The above tangerine peel pigment is applied to the formula of the popping bead wall material, wherein 4 parts of sodium alginate, 6 parts of agar, 3 parts of glycerol, 0.03 parts of tangerine peel pigment, V C 0.003 parts, the solvent is 100 parts of 0.2% acetic acid water. The prepared popping beads have uniform color, good stability, and a unique aroma of tangerine peel.

[0092] Embodiment 2:

[0093] (1) Select intact, high-quality tangerine peel raw materials, ensuring that they are fresh, dry and free of mold;

[0094] (2) taking the dried tangerine peel raw material of step (1), crushing it with a crusher, and passing it through a 40-mesh sieve to obtain dried tangerine peel powder;

[0095] (3) Weigh 50 g of tangerine peel powder, add 750 g of culture medium, inoculate 30% of Aspergillus oryzae strain, and ferment for 12 h at 30 °C and pH 7.0 to promote the release of pigment.

[0096] (4) The fermented mixture was placed in an ultrasonic extractor, with ethanol as the extraction solvent and a volume ratio of the fermentation mixture to ethanol of 1:5. Ultrasonic extraction was performed at 30°C for 20 minutes.

[0097] (5) After the ultrasonic treatment, the mixture was centrifuged at 4000 r / min for 5 min, and the supernatant was filtered through a 0.8 um filter membrane to remove the unreacted raw material residue and bacterial solution, i.e., the extract containing tangerine peel pigment.

[0098] (6) The extract was concentrated by rotary evaporation at 0.2 MPa and 40°C to 20% of the original volume to prepare tangerine peel pigment extract with a yield of 17.1%.

[0099] (7) The crude extract of tangerine peel pigment in step (6) was purified by separation using pretreated AB-8 macroporous resin, with the pH of the tangerine peel pigment solution adjusted to 7.0, the ethanol elution concentration being 60%, the sample volume being 250 mL, and the eluent volume being 150 mL to obtain a high-purity pigment product. The tangerine peel pigment had a purity of 69.4%.

[0100] (8) The purified tangerine peel pigment was freeze-dried in a freeze dryer at -20°C for 48 h. The sublimation and analytical drying temperatures were -30°C and 40°C, respectively, and the vacuum degrees were 55 Pa and 20 Pa, respectively. The tangerine peel pigment powder was collected and the pigment content was measured to be 8.6 g / 100 g.

[0101] The above tangerine peel pigment is applied to the formula of the popping bead wall material, wherein 3 parts of sodium alginate, 4 parts of agar, 2 parts of glycerin, 0.02 parts of tangerine peel pigment, V E 0.002 parts, the solvent is 80 parts of 0.5% acetic acid water. The prepared popping beads have stable color and slightly light tangerine peel aroma.

[0102] Comparative Example 1:

[0103] (1) Select intact, high-quality tangerine peel raw materials, ensuring that they are fresh, dry and free of mold;

[0104] (2) taking the dried tangerine peel raw material of step (1), crushing it with a crusher, and passing it through an 80-mesh sieve to obtain dried tangerine peel powder;

[0105] (3) Weigh 50 g of tangerine peel powder, add 1000 g of culture medium, inoculate 20% of yeast strain, and ferment at 25°C and pH 9.0 for 48 h to promote the release of pigment.

[0106] (4) The fermented mixture was placed in a round-bottom flask with a volume ratio of fermentation broth to ethanol solution of 1:5, and refluxed at 60°C for 2 h.

[0107] (5) After the extraction is completed, the mixture is centrifuged at 8000 r / min for 15 min, and the supernatant is filtered through a 1.0 um filter membrane to remove unreacted raw material residues and bacterial liquid, i.e., the extract containing tangerine peel pigment.

[0108] (6) The extract was concentrated by rotary evaporation at 0.5 MPa and 55°C to 20% of the original volume to prepare tangerine peel pigment extract with a yield of 9.6%.

[0109] (7) The crude extract of tangerine peel pigment in step (6) was purified by separation using pretreated D101 macroporous resin, with the pH of the tangerine peel pigment solution adjusted to 9.0, the ethanol elution concentration being 70%, the loading volume being 350 mL, and the eluent volume being 250 mL to obtain a high-purity pigment product. The tangerine peel pigment had a purity of 50.9%.

[0110] (8) The purified tangerine peel pigment was freeze-dried in a freeze dryer at -20°C for 36 h. The sublimation and analytical drying temperatures were -40°C and 40°C, respectively. The vacuum degrees were 60 Pa and 50 Pa, respectively. The tangerine peel pigment powder was collected and the pigment content was measured to be 1.1 g / 100 g.

[0111] The above tangerine peel pigment is applied to the formula of the popping pearl wall material, wherein 6 parts of sodium alginate, 8 parts of agar, 4 parts of glycerol, 0.04 parts of tangerine peel pigment, 0.004 parts of citric acid, and the solvent is 80 parts of 0.01% lactic acid water. The prepared popping pearls have a slightly lighter color, a slightly worse popping pearl stability, and a slightly lighter tangerine peel aroma.

[0112] Comparative Example 2:

[0113] (1) Select intact, high-quality tangerine peel raw materials, ensuring that they are fresh, dry and free of mold;

[0114] (2) taking the dried tangerine peel raw material of step (1), crushing it with a crusher, and passing it through an 80-mesh sieve to obtain dried tangerine peel powder;

[0115] (3) Weigh 50 g of tangerine peel powder, add 1000 g of culture medium, inoculate 20% of yeast strain, and ferment at 25°C and pH 9.0 for 48 h to promote the release of pigment.

[0116] (4) The fermented mixture was placed in an ultrasonic extractor, with ethanol as the extraction solvent and a volume ratio of the fermentation mixture to ethanol of 1:5. Ultrasonic extraction was performed at 30°C for 20 minutes.

[0117] (5) After the ultrasonic treatment, the mixture was centrifuged at 4000 r / min for 5 min, and the supernatant was filtered through a 0.8 um filter membrane to remove the unreacted raw material residue and bacterial solution, i.e., the extract containing tangerine peel pigment.

[0118] (6) The extract was concentrated by rotary evaporation at 0.2 MPa and 40°C to 20% of the original volume to prepare tangerine peel pigment extract with a yield of 17.1%.

[0119] (7) The crude extract of tangerine peel pigment in step (6) was purified by separation using pretreated ADS-7 macroporous resin, with the pH of the tangerine peel pigment solution adjusted to 9.0, the ethanol elution concentration being 70%, the loading volume being 350 mL, and the eluent volume being 250 mL to obtain a high-purity pigment product. The tangerine peel pigment had a purity of 32.5%.

[0120] (8) The tangerine peel pigment was freeze-dried in a freeze dryer at a temperature of -20°C and a freezing time of 36 h. The sublimation and analytical drying temperatures were -40°C and 40°C, respectively, and the vacuum degrees were 60 Pa and 50 Pa, respectively. The tangerine peel pigment powder was collected and the pigment content was measured to be 2.8 g / 100.

[0121] The above tangerine peel pigment is applied to the formula of the popping pearl wall material, wherein 6 parts of sodium alginate, 8 parts of agar, 4 parts of glycerol, 0.04 parts of tangerine peel pigment, 0.004 parts of citric acid, and the solvent is 80 parts of 0.01% lactic acid water. The prepared popping pearls are lighter in color, poor in popping pearl stability, and have a light tangerine peel aroma.

[0122] The test results of physical and chemical indicators of finished popping beads are as follows:

[0123]

[0124] The storage stability results of the popping beads are as follows:

[0125] Each popping bead sample was stored for a certain period of time, and its appearance was scored with a score range of 0-5.

[0126]

[0127] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A preparation process for tangerine peel pigment, characterized in that, The steps include: A) crushing tangerine peel to obtain tangerine peel powder; adding the tangerine peel powder to a fermentation medium, fermenting, and obtaining a fermented mixture; B) ultrasonically extracting the fermented mixture, centrifuging or filtering to obtain an extract containing orange peel pigment; C) The extract containing tangerine peel pigment is concentrated, purified by resin, and freeze-dried to obtain the product.

2. The preparation process according to claim 1, characterized in that: Step A) The pulverization is performed by passing the pulverized product through a 60-80 mesh sieve.

3. The preparation process according to claim 1, characterized in that: Step A) the microbial strains in the fermentation medium include Aspergillus oryzae and / or yeast, and the strain concentration is 5-30%; The solid-liquid ratio of the tangerine peel powder to the culture medium is 1:8-1:24; the fermentation temperature is 20-45°C, and the fermentation time is 12-48 hours; the initial pH value of the fermentation is adjusted to 5.0-9.0 using a buffer solution; the buffer solution can be a phosphate solution, a Tris buffer solution or a citric acid-sodium citrate solution.

4. The preparation process according to claim 1, characterized in that: Step B) The solvent of the ultrasonic extraction includes ethanol, acetone or ethyl acetate; the solid-liquid ratio of the ultrasonic extraction is 1:4-1:30; the temperature of the ultrasonic extraction is 30-60°C, and the time is 20-60 minutes.

5. The preparation process according to claim 1, characterized in that: Step B) the centrifugation parameters include 4000-8000 r / min, centrifugation for 5-15 min; The filter membrane used in the filtration is a nanofiltration membrane; the pore size of the filter membrane is 0.8-1 μm.

6. The preparation process according to claim 1, characterized in that: Step C) the concentration is rotary evaporation concentration, and the parameters of the rotary evaporation include 0.1-0.55Mpa, 40-65°C; The resin includes X-5, BM-2, AB-8 or D101; the pretreatment of the resin is as follows: soaking the resin in 95% ethanol for 24 to 48 hours to fully swell, rinsing with 95% ethanol, washing the ethanol with distilled water, soaking and rinsing with 1% to 5% HCL solution, washing with distilled water until neutral, then soaking and rinsing with 1% to 5% NaOH solution, and finally washing with distilled water until neutral for standby use; The static adsorption and desorption conditions of the resin are as follows: the pH of the extract containing tangerine peel pigment is 6.0~9.0, the ethanol elution concentration is 40%~70%, the sample volume is 200~350mL, and the eluent volume is 100~250mL.

7. The preparation process according to claim 1, characterized in that: Step C) The freeze-drying parameters include: Pre-freezing: Pre-freeze the orange peel pigment at -18 to -20°C for 24 to 48 hours; Sublimation drying: sublimation drying at -20 to -45°C for 12 to 24 hours, vacuum degree 45 to 80 Pa; Desorption drying: Desorption drying at 20-45°C for 4-6 hours, vacuum degree 10-50Pa.

8. A tangerine peel pigment, characterized in that The product is prepared by the preparation process described in any one of claims 1 to 7.

9. A bead-blasting wall material, characterized in that: The invention comprises the following raw materials in parts by weight: 3-6 parts of sodium alginate, 4-8 parts of agar, 2-4 parts of glycerin, 0.02-0.04 parts of tangerine peel pigment, 0.002-0.004 parts of VC, VE or citric acid, and 80-100 parts of solvent; The solvent is 0.1% to 0.5% acetic acid water or 0.01% to 0.2% lactic acid water.

10. A popping bead, characterized in that: Including the bursting bead wall material as described in claim 9.

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