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CN-116925785-B - Compound of gleditsia sinensis saponin and camellia saponin and preparation method thereof

CN116925785BCN 116925785 BCN116925785 BCN 116925785BCN-116925785-B

Abstract

The invention relates to the field of natural saponin separation and recombination, in particular to a compound of gleditsia sinensis saponin and camellia saponin and a preparation method thereof. The method comprises the steps of 1) respectively extracting gleditsia fruit peel and camellia cake to obtain crude gleditsia fruit saponin solution and crude camellia saponin solution, 2) respectively eluting the crude gleditsia fruit saponin solution and the crude camellia saponin solution by using macroporous adsorption resin AB-8 as a resin separation column, 3) respectively eluting the obtained gleditsia fruit saponin solution and the obtained camellia saponin solution by sequentially using 25-35% ethanol solution, 40-50% ethanol solution, 55-65% ethanol solution and 70-85% ethanol solution to obtain a gleditsia fruit saponin component and a camellia saponin component respectively, and 4) carrying out component recombination on the gleditsia fruit saponin component and the camellia saponin component to obtain a compound of gleditsia fruit saponin and camellia saponin. The invention can improve the purity of the natural saponin and the surface activity of the saponin, and overcomes the defect of higher critical micelle concentration of the sasanqua saponin.

Inventors

  • CHEN DIANSONG
  • JIANG JIANXIN
  • MA LING
  • MA SHIHONG
  • ZHU LIWEI

Assignees

  • 广州德谷个人护理用品有限公司
  • 北京林业大学

Dates

Publication Date
20260505
Application Date
20230704

Claims (9)

  1. 1. A preparation method of a compound of gleditsia sinensis saponin and camellia oleifera saponin is characterized by comprising the following steps: 1) Extracting fructus Gleditsiae Abnormalis pericarp with deionized water as extractant to obtain crude fructus Gleditsiae Abnormalis saponin solution, extracting oil tea cake with methanol as extractant, filtering, and drying to obtain crude oil tea saponin; 2) Macroporous adsorption resin AB-8 is used as a resin separation column, and the crude gleditsia sinensis saponin solution and the aqueous solution of crude tea-oil camellia saponin are respectively eluted to remove impurities; 3) Eluting the aqueous solution of the gleditsia sinensis saponin solution and the camellia oleifera saponin obtained in the step 2) with 25-35% ethanol solution, 40-50% ethanol solution, 55-65% ethanol solution and 70-85% ethanol solution respectively in sequence to obtain a gleditsia sinensis saponin component ZS30, a gleditsia sinensis saponin component ZS45, a gleditsia sinensis saponin component ZS60, a gleditsia sinensis saponin component ZS75, and a camellia oleifera saponin component YS25, a camellia oleifera saponin component YS45, a camellia oleifera saponin component YS65 and a camellia oleifera saponin component YS85 respectively; 4) And carrying out component recombination on at least one of the gleditsia sinensis saponin components ZS30, the gleditsia sinensis saponin component ZS45, the gleditsia sinensis saponin component ZS60 and the gleditsia sinensis saponin component ZS75 and at least one of the tea-oil camellia saponin components YS25, the tea-oil camellia saponin component YS45, the tea-oil camellia saponin component YS65 and the tea-oil camellia saponin component YS85 to obtain a composite of the gleditsia sinensis saponin and the tea-oil camellia saponin.
  2. 2. The preparation method of the compound of gleditsia sinensis saponin and camellia oleifera saponin according to claim 1, wherein in the step 1), gleditsia sinensis pericarp is crushed and screened by a 35-40 mesh sieve, deionized water is used as an extracting agent, the solid-liquid ratio is 1:8-10, stirring and extracting are carried out for 6-7 hours, and filtering is carried out to obtain crude gleditsia sinensis saponin solution; and/or crushing the oil tea cake, sieving with a 20-30 mesh sieve, taking methanol as an extracting agent, stirring and extracting for 6-7 h with a solid-liquid ratio of 1:4-6, filtering and drying to obtain crude oil tea saponin.
  3. 3. The method for preparing the compound of gleditsia sinensis saponin and camellia oleifera saponin according to claim 1, wherein in the step 2), deionized water and 10-15% ethanol solution are used for eluting sequentially.
  4. 4. The method for preparing the compound of gleditsia sinensis saponin and camellia oleifera saponin according to claim 3, wherein in the step 2), crude gleditsia sinensis saponin solution is loaded into macroporous adsorption resin AB-8, and is sequentially eluted by deionized water with the volume of 2-3 times of resin and 5-15% ethanol solution with the volume of 2-3 times of resin; And/or loading the aqueous solution of crude oil tea saponin into macroporous adsorption resin AB-8, and sequentially eluting with deionized water with the volume of 2-3 times of the resin volume and 5-15% ethanol solution with the volume of 2-3 times of the resin volume.
  5. 5. The method for preparing the compound of gleditsia sinensis saponin and camellia oleifera saponin according to claim 1, wherein in the step 3), for a crude gleditsia sinensis saponin solution, eluting with 30-35% ethanol solution, 45-50% ethanol solution, 55-60% ethanol solution and 70-75% ethanol solution in sequence to obtain a gleditsia sinensis saponin component ZS30, a gleditsia sinensis saponin component ZS45, a gleditsia sinensis saponin component ZS60 and a gleditsia sinensis saponin component ZS75; and/or eluting the aqueous solution of crude oil tea saponin with 25-30% ethanol solution, 40-45% ethanol solution, 60-65% ethanol solution and 75-85% ethanol solution in sequence to obtain oil tea saponin components YS25, YS45, YS65 and YS85.
  6. 6. The method for preparing a complex of sapogenin and sasanqua saponin according to claim 5, wherein in step 3), the 30-35% ethanol solution is 5-6 times the resin volume, the 45-50% ethanol solution is 10-12 times the resin volume, the 55-60% ethanol solution is 5-6 times the resin volume, the 70-75% ethanol solution is 2-3 times the resin volume, and/or, The volume of the 25-30% ethanol solution is 3-4 times of the volume of the resin, the volume of the 40-45% ethanol solution is 8-9 times of the volume of the resin, the volume of the 60-65% ethanol solution is 3-4 times of the volume of the resin, and the volume of the 75-85% ethanol solution is 1.5-2 times of the volume of the resin.
  7. 7. The method for preparing a complex of gleditsia sinensis saponin and camellia saponin according to any one of claims 1 to 6, wherein in step 4), the ratio of the gleditsia sinensis saponin component to the camellia saponin component is adjusted, so that the critical micelle concentration and the surface tension of the complex of gleditsia sinensis saponin and camellia saponin are adjustable.
  8. 8. The compound of the gleditsia sinensis saponin and the tea-oil saponin is characterized by being obtained by a preparation method of the compound of the gleditsia sinensis saponin and the tea-oil saponin according to any one of claims 1-7, wherein the compound of the gleditsia sinensis saponin and the tea-oil saponin is composed of a tea-oil saponin component YS25, a tea-oil saponin component YS45, a tea-oil saponin component YS65, a tea-oil saponin component YS85, a compound of a gleditsia sinensis saponin component ZS60 and a tea-oil saponin component ZS75 in a mass ratio of 1-3:30-32:18-22:1-3:2-3:1-3, or a compound of a gleditsia sinensis saponin component ZS30, a gleditsia sinensis saponin component ZS45, a gleditsia saponin component ZS60, a gleditsia saponin component ZS75, a tea-oil saponin component YS25 and a saponin component YS 75.
  9. 9. The complex of gleditsia sinensis saponin and camellia saponin of claim 8, wherein the complex of gleditsia sinensis saponin and camellia saponin has a surface tension of 34.6-41 mN/m and a critical micelle concentration of 0.1-1.5 g/L.

Description

Compound of gleditsia sinensis saponin and camellia saponin and preparation method thereof Technical Field The invention relates to the field of natural saponin separation and recombination, in particular to a compound of gleditsia sinensis saponin and camellia saponin and a preparation method thereof. Background Gleditsia sinensis (GLEDITISIA SINENSIS Lam.) Leguminosae Gleditsia are trees, up to 30 m, in the shape of fruit strips, 5-35 cm long, curved or straight, black brown or purple red, and multiple seeds, oblong, flat, about 1 cm long, and bright brown. The gleditsia sinensis is a multifunctional ecological economic tree species which is distributed all over the country and has a full bearing period of more than one hundred years. The gleditsia sinensis tree has developed root system, light preference, cold resistance, drought resistance, barren resistance, pollution resistance, disease and insect resistance and wide adaptability, is suitable for urban and rural landscape forests and road greening, can be used as a protective forest and a water and soil conservation forest tree species, and is listed in the national reserve forest tree species and yellow river basin ecological management ten tree species. The gleditsia sinensis polysaccharide has extremely high economic value, the gleditsia sinensis saponin is a high-quality natural surfactant, and the gleditsia sinensis saponin has the characteristics of environmental protection, no toxicity, biodegradability and the like, and has both economic value and ecological value. At present, the national gleditsia sinensis is planted the area exceeds 200 ten thousand mu. The oil tea (Camellia oleifera Abel) is a generic name of a plant with high grease content in camellia plants and cultivation economic value, and is called as 4 woody oil tree species in the world together with oil palm, olive and coconut. The Chinese has quite abundant oil tea resources, and mainly comprises more than 10 varieties of common oil tea, zhenhan camellia, zhejiang safflower oil tea, zhexian oil tea, small fruit oil tea, vietnam oil tea, japanese red camellia and the like. The camellia seed is provided with a shell, contains 50% -72% of kernel, 30% -40% of whole seed oil, 40% -60% of kernel oil, 8% -9% of crude protein, and the camellia oil is non-drying oil with unsaturated fatty acid content as high as 85% -97%, and is crown of various edible oils. Every 1 ton of tea oil is produced, and about 4 tons of tea cake and about 7 tons of tea shells are produced at the same time. The oil tea cake contains abundant saponin, and if the oil tea seeds can be fully developed and utilized, the economic benefit of the oil tea is 2-3 times of that of the pure tea oil. The oil tea is distributed in Yangtze river basin and south area in China, and the cultivation area is over 7000 ten thousand mu. The natural saponin is used as a surfactant and has the characteristics of environmental protection, no toxicity, biodegradability and the like. With the update and progress of people's living concept and the improvement of living standard, the daily detergent safety is more and more emphasized. However, for a long time, synthetic surfactants using fossil resources as raw materials have been the first choice for daily chemical detergents and cosmetics, and not only directly cause skin allergy and hair damage, but also accumulated chemical substances pollute the environment and harm the organisms in water, and the health of people is influenced along with food chains. The saponin is a natural surfactant, and does not bring negative problems of fluorescent agent, environmental hormone, river oxidation and the like. The use of renewable plant resources to produce degradable washing products is a necessary trend for human survival and development. At present, the problems of high purification cost, incomplete impurity removal, low surface activity of single natural saponin and the like still exist in the production process of the natural saponin. Disclosure of Invention In order to solve the technical problems, the invention provides a compound of gleditsia sinensis saponin and camellia oleifera saponin and a preparation method thereof. In a first aspect, the preparation method of the complex of gleditsia sinensis saponin and camellia oleifera saponin provided by the invention comprises the following steps: 1) Respectively extracting gleditsia sinensis peel and oil tea cake to obtain crude gleditsia sinensis saponin solution and crude oil tea saponin solution; 2) Macroporous adsorption resin AB-8 is used as a resin separation column, and the crude gleditsia sinensis saponin solution and the crude tea-oil camellia saponin solution are respectively eluted to remove impurities; 3) Eluting the gleditsia sinensis saponin solution and the camellia oleifera saponin solution obtained in the step 2) with 25-35% ethanol solution, 40-50% ethanol solution, 55-65% ethanol solution and 70-85% ethanol solution respectiv