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CN-122006289-A - Green technology for extracting natural ingredients of dried orange peel by water and application of green technology in beverage

CN122006289ACN 122006289 ACN122006289 ACN 122006289ACN-122006289-A

Abstract

The invention relates to a green process for extracting natural ingredients of dried orange peel by water and application of the green process in beverage. The process comprises the steps of crushing and drying a dried orange peel raw material, extracting the dried orange peel raw material with water at 105-125 ℃ and 0.8-1.5 MPa under a low oxygen condition to obtain a first extract and first-stage residues, extracting the residues at 130-150 ℃ and 1.5-2.2 MPa to obtain a second extract, treating the second extract at 145-165 ℃ and 1.8-2.5 MPa to obtain a low-ester pectin component containing combined flavone, mixing and homogenizing the first extract and the low-ester pectin component to disperse the volatile oil component in an aqueous phase containing the low-ester pectin component, and concentrating and/or drying the obtained dispersion to obtain the dried orange peel extract. The extract can be used as natural flavor additive for beverage.

Inventors

  • Lei Jiehua
  • CAI TINGWEI
  • LEI GUOTAI
  • CHEN JIAHAO
  • WEI GUOYING
  • BAI JUAN

Assignees

  • 泛亚香料(武汉)科技股份有限公司

Dates

Publication Date
20260512
Application Date
20260312

Claims (10)

  1. 1. A green process for extracting natural ingredients of dried orange peel by water is characterized by comprising the following steps: s1, crushing a dried orange peel raw material to 30-80 meshes, and drying until the moisture content is not more than 10%, so as to obtain pretreated dried orange peel; S2, under the condition of low oxygen, extracting the pretreated dried orange peel with water as an extraction solvent for 5-15 min at 105-125 ℃ and 0.8-1.5 MPa, leading out an extracting solution, cooling to 20-35 ℃, and carrying out solid-liquid separation to obtain a first extracting solution and first-stage residues; S3, extracting the residues in the first stage with water as an extraction solvent at 130-150 ℃ and 1.5-2.2 MPa for 8-20 min, and performing solid-liquid separation to obtain a second extract; S4, treating the second extracting solution for 2-8 min at 145-165 ℃ and 1.8-2.5 MPa, and cooling to 40-60 ℃ to obtain a low-ester pectin component containing combined flavone; S5, mixing the first extracting solution with the low-ester pectin component containing the combined flavone at the temperature of 45-60 ℃ and homogenizing to obtain an oil/water dispersion with the volatile oil component in the first extracting solution dispersed in a water phase; S6, concentrating and/or drying the oil/water dispersion to obtain the dried orange peel extract.
  2. 2. The green process according to claim 1, wherein the dried peel is dried ripe peel of citrus reticulata of the family rutaceae and cultivars thereof, and the extraction solvent is deionized water or purified water.
  3. 3. The green process according to claim 1, wherein the drying in S1 is 40-55 ℃ vacuum drying, the hypoxia condition in S2 is that the dissolved oxygen of the extraction water is not higher than 2 mg/L, and/or the top space of the extraction device is replaced by inert gas, and the extracted solution derived in S2 is cooled to 25-30 ℃ within 30S-3 min.
  4. 4. The green process according to claim 1, wherein the pectin content of the low-ester pectin component containing the combined flavone obtained in S4 is 40-90 wt%, the total flavone content is 0.5-15 wt%, the esterification degree of the pectin is 18-45%, and the weight average molecular weight is 30-150 kDa on a dry basis.
  5. 5. The green process according to claim 1, wherein S4 further comprises separating the cooled low-ester pectin component containing the combined-state flavone by an ultrafiltration membrane with a molecular weight cut-off value of 3-50 kDa, and collecting the cut-off liquid as the low-ester pectin component containing the combined-state flavone for S5.
  6. 6. The green process according to claim 1, wherein the mass ratio of the volatile oil component in the first extract to the pectin in the low-ester pectin component containing the combined flavone in S5 is 1 (2-30), the homogenizing treatment is high-pressure homogenizing or micro-jet homogenizing, the homogenizing pressure is 10-80 MPa, and the volume average particle size D50 of the oil/water dispersion obtained in S5 is 0.1-0.8 μm.
  7. 7. The dried orange peel extract is prepared by the green process according to any one of claims 1-6, is an aqueous dispersion, a concentrate or a dried product thereof, and comprises an orange peel volatile oil component and a low-ester pectin component containing combined flavones, wherein the orange peel volatile oil component is dispersed in an oil drop form in an aqueous continuous phase containing the low-ester pectin component.
  8. 8. The dried orange peel extract according to claim 7, wherein the dried orange peel extract is reconstituted with water to form a dispersion having a volume average particle diameter D50 of 0.1-0.8 μm and a polydispersity index PDI of not more than 0.35 at a pH of 2.8-4.2, and the flavonoid compound in the combined flavonoid is one or more selected from hesperidin, nobiletin, hesperetin and naringenin.
  9. 9. Use of the dried orange peel extract according to claim 7 or 8 for the preparation of a natural flavour additive for beverages.
  10. 10. A beverage comprising the dried orange peel extract according to claim 7 or 8, wherein the dried orange peel extract is added to the beverage in an amount of 0.03-0.12 wt%, and the pH of the beverage is 2.8-4.2.

Description

Green technology for extracting natural ingredients of dried orange peel by water and application of green technology in beverage Technical Field The invention belongs to the technical field of natural product extraction and application, and particularly relates to a green process for extracting natural ingredients of dried orange peel by water and application of the green process in beverage. Background The pericarpium Citri Tangerinae is dried mature pericarp of Citrus reticulata Blanco (Citrus reticulata Blanco) of Rutaceae and its cultivar, and is a traditional Chinese medicinal material and natural flavoring material. The pharmacopoeia records that the outer surface of the dried orange peel medicinal material is provided with a punctiform oil chamber, and components such as hesperidin, nobiletin, hesperetin and the like are used as quality control indexes. Modern researches also show that the citrus peel is rich in volatile oil, flavone, pectin and other functional components, and has high development value of food and health products. The traditional tangerine peel extraction method mainly comprises a steam distillation method, an organic solvent extraction method, a supercritical CO 2 extraction method and the like, but the steam distillation method has low yield and is difficult to consider nonvolatile components, the organic solvent extraction method has the risk of solvent residue, and the supercritical CO 2 extraction method has high equipment investment and is difficult to extract polar components such as pectin and the like efficiently. The method is difficult to realize the low-temperature protective extraction of the volatile oil and the high-temperature release and structure regulation of the pectin-flavone component in a single process flow. The subcritical water extraction technology utilizes the characteristic that the dielectric constant of water at high temperature and high pressure is reduced along with the temperature rise, the polarity of the solvent can be changed by adjusting the temperature and the pressure, the selective extraction of components with different polarities is realized, and the whole process takes water as the solvent, so that the method accords with the development trend of green chemistry. In the prior art, there is a report of extracting citrus raw materials by subcritical water, and as disclosed in CN102526295A, a method for comprehensively utilizing dried orange peel is disclosed. However, the method aims at single component extraction, or relies on a subsequent organic solvent for carrying out distribution extraction, or relies on membrane separation to realize component separation after single temperature extraction, and the method has the defects that in-situ regulation and control on the esterification degree and molecular weight of pectin are lacking, low-ester pectin with an emulsifying function cannot be synchronously prepared in the extraction process, the oxygen content of the volatile oil extraction environment is lack of control, the thermal oxidation deterioration risk is high, the extracted volatile oil and pectin are respectively collected as independent products, in-situ emulsification package of the volatile oil cannot be realized, and the dispersion stability of the obtained extract in an aqueous beverage system is insufficient. In addition, in the end application of beverages and the like, the tangerine peel volatile oil is extremely easy to delaminate in an aqueous phase system due to water insolubility, and the prior art is lack of an integrated process which is suitable for acid beverages and is formed by directly emulsifying the self volatile oil of the homologous pectin obtained by in-situ regulation and control of the tangerine peel raw material, the whole aqueous phase and subcritical water. Therefore, the development of the green extraction process for the dried orange peel, which takes water as a solvent in the whole process and synchronously realizes the pectin de-esterification modification and the volatile oil in-situ emulsification encapsulation in the extraction process, has great significance for preparing the high-quality dried orange peel extract which can be directly applied to the field of beverages. Disclosure of Invention The first object of the present invention is to provide a green process for extracting natural ingredients of dried orange peel with water, wherein the process combines gradient temperature and pressure graded extraction and in-situ emulsification, and only uses water as solvent in the whole process, thereby synchronously realizing the low-oxygen protective extraction of volatile oil, subcritical hydrothermal de-esterification modification of pectin and in-situ emulsification encapsulation of volatile oil in the extraction process, and the obtained dried orange peel extract can be directly applied to an aqueous beverage system. The second object of the present invention is to provide the dried orange peel