WO2020061891A1 - 一种柑橘源复合益生元制剂的制备方法与应用 - Google Patents

一种柑橘源复合益生元制剂的制备方法与应用 Download PDF

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WO2020061891A1
WO2020061891A1 PCT/CN2018/107919 CN2018107919W WO2020061891A1 WO 2020061891 A1 WO2020061891 A1 WO 2020061891A1 CN 2018107919 W CN2018107919 W CN 2018107919W WO 2020061891 A1 WO2020061891 A1 WO 2020061891A1
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orange
acid
citrus
solution
petals
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PCT/CN2018/107919
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French (fr)
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陈士国
郑家琪
叶兴乾
刘东红
张华�
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浙江大学
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Priority to PCT/CN2018/107919 priority Critical patent/WO2020061891A1/zh
Priority to US16/754,137 priority patent/US11110143B2/en
Publication of WO2020061891A1 publication Critical patent/WO2020061891A1/zh

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/01—Instant products; Powders; Flakes; Granules
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/03—Products from fruits or vegetables; Preparation or treatment thereof consisting of whole pieces or fragments without mashing the original pieces
    • A23L19/07—Fruit waste products, e.g. from citrus peel or seeds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • A23L2/04—Extraction of juices
    • A23L2/06—Extraction of juices from citrus fruits
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/135—Bacteria or derivatives thereof, e.g. probiotics
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/30—Dietetic or nutritional methods, e.g. for losing weight
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/75—Rutaceae (Rue family)
    • A61K36/752—Citrus, e.g. lime, orange or lemon
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/08—Solutions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
    • A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction

Definitions

  • the invention belongs to the field of comprehensive utilization of canned fruit and vegetable production wastewater, and particularly relates to a preparation method and application of a citrus source composite prebiotic preparation.
  • Citrus has a large output and a large area, and is one of the most important cash crops and international agricultural products and processed products. China's citrus production ranks among the highest in the world, and most of it is broad-skinned citrus and grapefruit. The rich source of raw materials makes China a major country for citrus processing, especially canned orange slices. Due to the unique varieties of Chinese citrus and relatively cheap labor, Chinese canned citrus products have unique advantages in the world, accounting for 70-80% of the total international market share, and are increasing year by year. In the process of canned citrus processing, the orange capsules must be removed, and the orange capsules are treated with acid water and alkaline water to remove the capsules. During this process, a large amount of discharged water in which the coating components are dissolved will be generated.
  • the discharged water contains a large amount of acid residues, alkali residues, organic matter, and the COD value and BOD value greatly exceed environmental protection requirements.
  • most of the methods are processed by precipitating pectin after adjusting the pH and blasting after pressing. This method has a high processing cost, and pectin slag cannot be directly stacked.
  • Canned citrus processing enterprises consume a lot of water. According to the "Canned Industry Manual," producing 1 ton of canned syrup and orange slices can consume 60 tons of water. After technological transformation, most enterprises have more than 30 tons, with large emissions and high processing costs.
  • the acid-base treatment discharge water is rich in pectin, flavonoids, oligosaccharides, other fibers and other prebiotics, which has the function of reversing the intestinal flora disorder. Fully recycling them can obtain high-value prebiotic products. At the same time, It also solves the problem of the discharge of acid-base treated water and generates huge social and environmental benefits. Citrus tangerine petals are covered by citrus peel, and there is no risk of pesticide residue or chemical pollution. Acid and alkali solutions are used to soak the orange petals to avoid the risk of microbial contamination. Therefore, the obtained acid-base treated water is highly safe for recycling.
  • the purpose of the present invention is to rapidly prepare a citrus source compound prebiotic preparation by using acid-base decapsulation treatment and discharged water as raw materials in canned citrus processing.
  • the key step of the method is to use an acid solution such as citric acid and an alkali solution such as potassium hydroxide and sodium hydroxide to sequentially treat the orange petals to remove the capsule.
  • an acid solution such as citric acid
  • an alkali solution such as potassium hydroxide and sodium hydroxide
  • the present invention uses a simple operation unit to obtain a composite prebiotic product with intestinal probiotic functions at a lower cost from citrus processed water, which is expected to obtain certain economic benefits, and is a perfect complement to the citrus processing comprehensive utilization process. It solves the problem of citrus processed water discharge and produces certain social benefits.
  • the acid-treated orange petals are transferred to an alkaline solution, and the orange petals are treated with a certain volume of alkaline solution, the alkali solution concentration is greater than 0.1g / 100ml, soaked until the orange petal capsule coating is dissolved, and the alkali-treated water is obtained after filtration;
  • the acid-treated water or the acid-adjusted alkali-treated water is adjusted to a pH of 4-7, and a composite prebiotic preparation is obtained after filtering.
  • citrus is selected from citrus plants, including but not limited to broad-skinned citrus, pomelo, orange, grapefruit, lemon.
  • acids used include, but are not limited to, food-grade hydrochloric acid, citric acid, oxalic acid, tartaric acid, malic acid, and lactic acid.
  • the ratio of the orange petal and the acid solution is 1g: 1ml-1g: 5ml.
  • the base used includes, but is not limited to, food-grade NaOH, Na 2 CO 3 , KOH, K 2 CO 3 , Mg (OH) 2 , Ca (OH) 2 .
  • the ratio of the orange petal and the alkaline solution is 1g: 1ml-1g: 5ml.
  • the concentration of the alkali solution used is 0.4-0.8g / 100ml
  • the processing temperature is 5-80 ° C
  • the processing time is 10-15min.
  • the above preparation is used for preparing prebiotic oral liquid, prebiotic powder, and health products for reversing intestinal flora disturbance caused by antibiotics.
  • the preparation method of the composite prebiotic powder is as follows: the citrus source composite prebiotic preparation is spray-dried to obtain the citrus source composite prebiotic powder.
  • the beneficial effect of the invention is that a complex prebiotic product with intestinal probiotic function and efficacy is obtained from the citrus processed water at a lower cost using a simple operation unit. Has the following characteristics:
  • the raw material of the product is citrus processing water, which has low product cost and good safety;
  • the processing process is the improvement of the comprehensive utilization of citrus processing wastewater, which greatly reduces the COD value of the discharged water and has good social benefits;
  • the product contains a variety of prebiotics such as pectin, flavones, oligosaccharides, and other fibers.
  • prebiotics such as pectin, flavones, oligosaccharides, and other fibers.
  • the synergistic effect of each component can effectively reverse the intestinal flora disorder caused by antibiotics.
  • the pectin component in the product has the functions of reducing serum cholesterol content, controlling blood sugar content, preventing allergies, preventing the occurrence and metastasis of cancer, and helping to eliminate heavy metal elements in the body.
  • Flavonoids have functions of lowering blood lipids, anti-allergy, anti-cancer, anti- Viruses, anti-inflammation, bacteriostasis, strengthening of capillaries and other functions, oligosaccharides have functions of intestinal laxative, lowering serum cholesterol content, other fibers have functions of controlling weight, preventing bowel cancer and constipation, lowering blood lipids, controlling blood sugar and other functions.
  • Figure 1 is a standard curve for flavonoid content
  • Figure 2 is a standard curve for oligosaccharide content
  • FIG. 3 Distribution of horizontal genera in the genus.
  • C stool before experiment
  • AC control stool after 1 week of irrigation
  • AA stool of model group after 1 week of antibiotics
  • TC stool of 2 weeks after control
  • TA stool of 2 weeks after model
  • TP Feces of the model group 2 weeks after gavage.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • Treat the orange petals with a citric acid solution with a concentration of 0.4g / 100ml.
  • the ratio of orange petals to acid water is 1g: 1ml.
  • the stirring keep stirring the solution to ensure that the acid and orange petals are in full contact. It should be noted that the stirring should not be too intense, so as not to break the orange petals.
  • the acid-treated water was used to adjust the alkali-treated water to a pH of the mixed solution of 7 to obtain a composite prebiotic oral solution. Under the treatment conditions, there are less precipitates in the oral solution, and the integrity of the orange petals obtained by the treatment is good.
  • the flavonoid content analysis was based on the sodium nitrite method. 25mg of hesperidin was dissolved in 0.4g / L sodium hydroxide solution, and the volume was adjusted to 50mL. Prepare standard sample solutions with concentrations of 0, 50, 100, 150, 200, and 250 ⁇ g / mL in this order. Take 1mL of the standard sample solution and add 4mL of 0.4g / L sodium hydroxide solution to obtain 5mL of the reaction solution.
  • reaction solution to a water bath at 80 ° C, add 0.6 mL of 5% sodium nitrite solution, mix well, add 0.6 mL of 10% sodium nitrate solution, mix well, add 1 mol / L 80 ° C sodium hydroxide solution, 4 mL, and bath in 80 ° C for 10 min.
  • a blank solution prepared by using 1 mL of the above-mentioned 0.4 g / L sodium hydroxide solution as a reference was used, and its absorbance was measured at a wavelength of 356 nm.
  • oligosaccharides The analysis of oligosaccharides is based on the phenol-sulfuric acid method. After the macromolecular polysaccharides are removed by oral liquid alcohol precipitation, the sugars contained in the samples are all oligosaccharides. This method can be used to determine the product oligosaccharides. Take 20mg of glucose, dissolve in water and make up to 100mL. Prepare standard sample solutions with concentrations of 0, 20, 40, 60, 80, and 100 ⁇ g / mL in this order. Take 2mL of standard sample solution, add 1mL of 5% phenol solution (new), mix well, add 8mL of concentrated sulfuric acid, mix immediately, keep in a boiling water bath for 20min, take it out, and cool in a cold water bath.
  • the absorbance of each solution was measured at a wavelength of 490nm, the concentration of the glucose dilution solution ( ⁇ g / ml) was used as the abscissa, and the absorbance was used as the ordinate. 2.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • Treat the orange petals with a citric acid solution with a concentration of 0.8g / 100ml.
  • the ratio of orange petals to acid water is 1g: 5ml.
  • keep stirring the solution to ensure that the acid and orange petals are in full contact. It should be noted that the stirring should not be too intense, so as not to break the orange petals.
  • the acid-treated water was used to adjust the alkali-treated water to a pH of the mixed solution of 7 to obtain a composite prebiotic oral solution. Under the treatment conditions, there are less precipitates in the oral solution, and the integrity of the orange petals obtained by the treatment is good.
  • pectin content was measured according to the measurement method of Example 1.
  • the measurement results were as follows: pectin content 475.00 ⁇ g / mL, flavonoid content 71.24 ⁇ g / mL, and oligosaccharide content 205.10 ⁇ g / mL.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • the orange petals were treated with a citric acid solution with a concentration of 0.05g / 100ml, the ratio of orange petals to acid water was 1g: 1ml, and the treatment was performed at 5 ° C for 10min.
  • the solution was continuously stirred to ensure that the acid solution and the orange petals were in full contact. It should be noted that the stirring should not be too intense, so as not to break the orange petals.
  • pectin content 972.00 ⁇ g / mL
  • flavonoid content 223.89 ⁇ g / mL
  • oligosaccharide content 698.43 ⁇ g / mL.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • Treat the orange petals with a citric acid solution with a concentration of 1g / 100ml.
  • the ratio of orange petals to acid water is 1g: 5ml.
  • keep stirring the solution to ensure that the acid and orange petals are in full contact. Note that the stirring should not be too intense, so as not to break the orange petals.
  • pectin content, flavonoid content, and oligosaccharide content were measured according to the measurement method of Example 1.
  • the measurement results were as follows: pectin content 630.56 ⁇ g / mL, flavonoid content 114.78 ⁇ g / mL, and oligosaccharide content 476.78 ⁇ g / mL.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • Treat the orange petals with a citric acid solution with a concentration of 0.6g / 100ml.
  • the ratio of orange petals to acid water is 1g: 1.5ml.
  • the stirring keep stirring the solution to ensure that the acid and orange petals are in full contact.
  • the stirring should not be too intense, so as not to break the orange petals.
  • pectin content 1125.47 ⁇ g / mL
  • flavonoid content 204.39 ⁇ g / mL
  • oligosaccharide content 475.21 ⁇ g / mL.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • Treat the orange petals with a citric acid solution with a concentration of 0.6g / 100ml.
  • the ratio of orange petals to acid water is 1g: 1.5ml.
  • the stirring keep stirring the solution to ensure that the acid and orange petals are in full contact.
  • the stirring should not be too intense, so as not to break the orange petals.
  • the acid-treated water was used to adjust the alkali-treated water to a mixed solution pH of 7, and the mixed solution was spray-dried to obtain a composite prebiotic powder.
  • the product had a pectin content of 40-60%, a flavonoid content of 10-20%, and an oligosaccharide content. 30-40%.
  • the citrus is treated in the boiling water for 0.5 min, so that the orange peel, the orange tangerine peel and the orange petal of the citrus can be more easily separated.
  • the citrus after the boiling water treatment removes the orange peel and tangerine while it is still hot.
  • Treat the orange petals with a citric acid solution with a concentration of 0.6g / 100ml.
  • the ratio of orange petals to acid water is 1g: 1.5ml.
  • the stirring keep stirring the solution to ensure that the acid and orange petals are in full contact.
  • the stirring should not be too intense, so as not to break the orange petals.
  • the powder has the function of reversing the disturbance of intestinal flora.
  • a mouse model of intestinal flora imbalance was produced by intragastric administration of a broad spectrum of antibiotics, and a normal control group and a powder intervention group were also set up. 16SRNA sequencing was performed on the tested mouse flora, and OTU analysis and species analysis, principal component analysis, and significance analysis of differences in community structure between groups were performed.
  • the intestinal flora diversity of the mice in the powder intervention group increased significantly and was similar to that in the normal control group, indicating that the powder intervention can reverse the mice's intestinal flora disturbance caused by antibiotics.
  • the relative abundance of beneficial bacteria such as Bifidobacterium and Bacteroides in the powder intervention group was also significantly increased, while the abundance of harmful bacteria such as Paeruginosa (Pseudomonas aeruginosa) and Escherichia-Shigella (Escherichia coli Shigella) was significantly reduced.
  • beneficial bacteria such as Bifidobacterium and Bacteroides
  • harmful bacteria such as Paeruginosa (Pseudomonas aeruginosa) and Escherichia-Shigella (Escherichia coli Shigella) was significantly reduced.

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Abstract

公开了一种柑橘源复合益生元制剂的制备方法及该制剂的用途，包括如下步骤：热水漂烫柑橘后剥除外橘皮，分瓣后使用酸溶液和碱溶液浸泡橘瓣脱除其囊衣，所得碱浸泡水用酸浸泡水或者酸调节pH至弱酸性到中性后，过滤即可得到复合型益生元制剂。该制剂具有逆转肠道菌群紊乱的功能，该方法具有操作简单、成本低的特点。

Description

一种柑橘源复合益生元制剂的制备方法与应用 技术领域
本发明属于果蔬罐头生产废水综合利用领域，尤其涉及一种柑橘源复合益生元制剂的制备方法与应用。
技术背景
柑橘产量大，种植面积广，是最重要的经济作物和国际农产品与加工品之一。中国柑橘产量常年居世界前列，且大部分为宽皮柑橘和柚子，丰富的原料来源使中国成为柑橘加工的主要国家，特别是糖水橘片罐头。由于中国柑橘品种独特，劳动力相对便宜，中国的柑橘罐头产品在世界上具有独一无二的优势，占国际市场总份额的70-80％，并且逐年增加。柑橘罐头加工过程中，必须脱除橘瓣囊衣，生产上使用酸水处理和碱水处理橘瓣去除囊衣。这一处理过程中会产生溶有大量囊衣成分的排放水，排放水中含有大量酸残留、碱残留、有机物，COD值和BOD值大大超出环保要求。目前大部分采用调pH处理后沉淀果胶、压榨后经爆气处理的方法进行处理，此种方法处理费用高，果胶压榨渣无法直接堆放。柑橘罐头加工企业耗水量大，按照《罐头工业手册》生产1吨糖水橘片罐头需要耗水60吨，经技术改造后大部分企业在30吨以上，排放量大，处理费用高。
酸碱处理排放水中富含果胶、黄酮类、低聚糖、其他纤维等益生元，具有逆转肠道菌群紊乱的功能，将其进行全回收利用既可得到高价值的益生元产品，同时也解决了酸碱处理水的排放问题，产生巨大的社会和环境效益。柑橘橘瓣均由柑橘皮包裹，本身无农药残留、化学污染等风险。酸溶液和碱溶液对橘瓣进行浸泡处理，避免了微生物污染的风险。因此，得到的酸碱处理水进行回收利用的安全性高。
发明内容
本发明的目的在于以柑橘罐头加工中酸碱脱囊衣处理排放水为原料，快速制备一种柑橘源复合益生元制剂。该方法关键工序为使用柠檬酸等酸溶液和氢氧化钾、氢氧化钠等碱溶液先后处理橘瓣以去除其囊衣。用酸处理水或酸调节碱处理水至弱酸性到碱性，即可得到富含果胶、黄酮类、低聚糖以及其他纤维的复合型益生元功能制剂。本发明使用简单的操作单元从柑橘加工水中以较低的成本得到具有肠道益生功能功效的复合型益生元产品，预期获得一定的经济收益，是对柑橘加工综合利用工艺的填补完善，同时也解决了柑橘加工水的排 放问题，产生一定的社会效益。
本发明的目的是通过以下技术方案实现的：一种柑橘源复合益生元制剂的制备方法，包括如下步骤：
(4)用一定体积酸溶液处理柑橘橘瓣，酸溶液浓度大于0.05g/100ml，浸泡处理直到橘瓣囊衣呈凝胶状，过滤橘瓣，得到酸处理水；
(5)将酸处理过的橘瓣转移到碱溶液中，用一定体积碱溶液处理橘瓣，碱溶液浓度大于0.1g/100ml，浸泡处理直到橘瓣囊衣溶解，过滤后得到碱处理水；
(6)用酸处理水或者酸调节碱处理水pH至4-7，过滤后得到复合型益生元制剂。
进一步地，所述柑橘选自柑橘属植物，包括但不限于宽皮柑橘、柚、橙、葡萄柚、柠檬。
进一步地，所用的酸包括但不限于食品级的盐酸、柠檬酸、草酸、酒石酸、苹果酸、乳酸。
进一步地，橘瓣和酸溶液的比例为1g:1ml-1g:5ml。
根据权利要求1中所述的方法，其特征在于，酸溶液浓度为0.4-0.8g/100ml，处理温度为5-80℃，处理时间为20-40min。
进一步地，所用的碱包括但不限于食品级的NaOH、Na 2CO 3、KOH、K 2CO 3、Mg(OH) 2、Ca(OH) 2。
进一步地，橘瓣和碱溶液的比例为1g:1ml-1g:5ml。
进一步地，所用碱溶液浓度为0.4-0.8g/100ml，处理温度为5-80℃，处理时间为10-15min。
上述制剂在制备益生元口服液、益生元粉剂、以及逆转抗生素引起的肠道菌群紊乱的保健品中的应用。
复合益生元粉剂的制备方法为：将柑橘源复合益生元制剂进行喷雾干燥后得到所述柑橘源复合益生元粉剂。
本发明的有益效果在于：使用简单的操作单元从柑橘加工水中以较低的成本得到具有肠道益生功能功效的复合型益生元产品。具有以下特点：
(1)无需进行特殊的脱盐工艺，通过简单操作单元直接得到产品；
(2)产品原料为柑橘加工处理水，产品成本低、安全性好；
(3)加工过程为柑橘加工废水综合利用的完善，大大降低排放水COD值，有很好的社会效益；
(4)是一种复合型的益生元产品，产品中含有果胶、黄酮、低聚糖、其他纤维等多种益生元，各组分协同作用可以有效逆转抗生素导致的肠道菌群紊乱。 除此之外，产品中果胶成分具有降低血清胆固醇含量、控制血糖含量、预防过敏症、预防癌症发生与转移、帮助体内重金属元素排除等功能，黄酮具有降血脂、抗过敏、抗癌、抗病毒、消炎、抑菌、强化毛细血管等功能，低聚糖具有润肠通便、降低血清胆固醇含量等功能，其他纤维具有控制体重、预防肠癌与便秘、降低血脂、控制血糖等功能。
附图说明
图1为黄酮含量标准曲线；
图2为低聚糖含量标准曲线；
图3属水平菌群分布图。其中，C：实验开始之前的粪便，AC：灌水1周后的对照粪便，AA：灌抗生素一周后的模型组粪便，TC：对照组2周之后的粪便，TA：模型组2周之后的粪便，TP：模型组灌胃粉剂2周之后的粪便。
具体实施方式
实施例1
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为0.4g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:1ml，在20℃处理20min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。
将酸处理过的橘瓣分别加入到浓度为0.4g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:1ml的比例处理橘瓣，30℃处理10min，处理过程中应不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。
用酸处理水调节碱处理水至混合液pH为7，得到一种复合型益生元口服液。该处理条件下口服液中沉淀物较少，处理得到的橘瓣完整度好。
对得到的复合型益生元口服液果胶含量、黄酮含量、低聚糖含量进行测定：
果胶含量
取口服液150mL，向试样中按乙醇与试样体积比1:1加入95％乙醇，于室温条件下沉淀2h。将试样乙醇沉淀液转移入300目滤袋中进行过滤，用95％乙醇15mL洗涤残渣2次，过滤方法同上。将滤渣用刮勺转移至坩埚中，将坩埚连同滤渣在50℃烘干6h，待滤渣干燥至恒重后测定其质量。测得该口服液果胶含量为1144.00μg/mL。
黄酮含量
黄酮含量分析基于亚硝酸钠法。取25mg橙皮苷溶于0.4g/L氢氧化钠溶液中，定容至50mL。依次配成浓度为0、50、100、150、200、250μg/mL标准样品溶液。取标准样品溶液1mL，加入0.4g/L氢氧化钠溶液4mL，得到反应液5mL。将反应液80℃水浴，加入5％亚硝酸钠溶液0.6mL，混匀，加入10％硝酸钠溶液0.6mL，混匀，加入1mol/L 80℃氢氧化钠溶液4mL，于80℃水浴10min，待冷却后以上述0.4g/L氢氧化钠溶液1mL所制得的空白溶液做参比，于356nm波长处测定其吸光度。以橙皮苷浓度(μg/mL)为横坐标，吸收度为纵坐标，绘制标准曲线，见图1，计算得回归方程为y＝326.55x+0.096，R 2＝0.999。取样品1mL以相同方法测定其吸光度值，并利用标准曲线计算其黄酮含量。测定该口服液黄酮含量为237.66μg/mL。
低聚糖含量
低聚糖分析基于苯酚-硫酸法，由于口服液醇沉除去大分子多糖后，样品所含糖类均为低聚糖，可使用该法对产品低聚糖进行测定。取葡萄糖20mg，用水溶解并定容至100mL。依次配成浓度为0、20、40、60、80、100μg/mL标准样品溶液。取标准样品溶液2mL，加入5％苯酚溶液(新制)1mL，混匀，加入浓硫酸8mL，立即混匀，于沸水浴中保温20min，取出，置冷水浴中冷却。以上述2mL水所制得的空白溶液做参比，于490nm波长处测定各溶液吸光度，以葡萄糖稀释液的浓度(μg/ml)为横坐标，吸收度为纵坐标，绘制标准曲线，见图2，计算得回归方程为y＝112.42x-1.5083，R 2＝0.997。取样品稀释液2mL以相同方法测定其吸光度值，并利用标准曲线计算其低聚糖含量。测定该口服液低聚糖含量为282.37μg/mL。
实施例2
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为0.8g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:5ml，在30℃处理40min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。
将酸处理过的橘瓣分别加入到浓度为0.8g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:5ml的比例处理橘瓣，40℃处理15min，处理过程中应不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。
用酸处理水调节碱处理水至混合液pH为7，得到一种复合型益生元口服液。该处理条件下口服液中沉淀物较少，处理得到的橘瓣完整度好。
按实施例1的测定方法对其果胶含量、黄酮含量、低聚糖含量进行测定，测得结果如下：果胶含量475.00μg/mL，黄酮含量71.24μg/mL，低聚糖含量205.10μg/mL。
实施例3
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为0.05g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:1ml，在5℃处理10min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。将酸处理过的橘瓣分别加入到浓度为0.1g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:1.5ml的比例处理橘瓣，5℃处理5min，处理过程中应不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。用酸处理水调节碱处理水至混合液pH为7，得到一种复合型益生元口服液。该处理条件下口服液中沉淀物少，处理得到的橘瓣完整度好。
按实施例1的测定方法对其果胶含量、黄酮含量、低聚糖含量进行测定，测得结果如下：果胶含量972.00μg/mL，黄酮含量223.89μg/mL，低聚糖含量698.43μg/mL。
实施例4
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为1g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:5ml，在80℃处理60min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。将酸处理过的橘瓣分别加入到浓度为1g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:1.5ml的比例处理橘瓣，80℃处理60min，处理过程中应不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。用酸处理水调节碱处理水至混合液pH为7，得到一种复合型益生元口服液。
按实施例1的测定方法对其果胶含量、黄酮含量、低聚糖含量进行测定，测得结果如下：果胶含量630.56μg/mL，黄酮含量114.78μg/mL，低聚糖含量476.78μg/mL。
实施例5
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为0.6g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:1.5ml，在28℃处理30min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。将酸处理过的橘瓣分别加入到浓度为0.6g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:1.5ml的比例处理橘瓣，32℃处理10min，处理过程中应不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。用柠檬酸调节碱处理水至混合液pH为7，得到一种复合型益生元口服液。
按实施例1的测定方法对其果胶含量、黄酮含量、低聚糖含量进行测定，测得结果如下：果胶含量1125.47μg/mL，黄酮含量204.39μg/mL，低聚糖含量475.21μg/mL。
实施例6
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为0.6g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:1.5ml，在28℃处理30min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。将酸处理过的橘瓣分别加入到浓度为0.6g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:1.5ml的比例处理橘瓣，32℃处理10min，处理过程中应不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。用酸处理水调节碱处理水至混合液pH为7，混合液进行喷雾干燥得到一种复合型益生元粉剂，产品中果胶含量40-60％，黄酮含量10-20％，低聚糖含量30-40％。
实施例7
本实施例将柑橘放入沸水中处理0.5min，可使柑橘的橘皮和橘络与橘瓣更易分离。沸水处理后的柑橘趁热除去橘皮和橘络。以浓度为0.6g/100ml的柠檬酸溶液处理橘瓣，橘瓣与酸水的比例为1g:1.5ml，在28℃处理30min，处理过程中不断搅拌溶液以保证酸液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。将酸处理过的橘瓣分别加入到浓度为0.6g/100ml的碳酸钠溶液中，以橘瓣：碱水＝1g:1.5ml的比例处理橘瓣，32℃处理10min，处理过程中应 不断搅拌溶液以保证碱液和橘瓣充分接触，但需要注意搅拌不宜过于激烈，以免橘瓣破碎。用酸处理水调节碱处理水至混合液pH为7，混合液进行冻干得到一种复合型益生元粉剂。
该粉剂具有逆转肠道菌群紊乱的功能。通过广谱抗生素灌胃制造肠道菌群失衡小鼠模型，同时设置正常对照组和粉剂干预组。对受试小鼠菌群进行16SRNA测序，并进行OTU分析和物种分析、主成分分析、组间群落结构差异显著性分析等。粉剂干预组小鼠的肠道菌群多样性显著增加且与正常对照组相近，说明粉剂干预可以逆转抗生素引起的小鼠肠道菌群紊乱。粉剂干预组小鼠的双歧杆菌、拟杆菌等有益菌的相对丰度也显著提高，而有害菌如Paeruginosa(绿脓杆菌)和Escherichia-Shigella(大肠杆菌志贺菌)的丰度显著减少。

Claims (10)

  1. 一种柑橘源复合益生元制剂的制备方法，其特征在于，包括如下步骤：
    (1)用一定体积酸溶液处理柑橘橘瓣，酸溶液浓度大于0.05/100ml，浸泡处理直到橘瓣囊衣呈凝胶状，过滤橘瓣，得到酸处理水；
    (2)将酸处理过的橘瓣转移到碱溶液中，用一定体积碱溶液处理橘瓣，碱溶液浓度大于0.1/100ml，浸泡处理直到橘瓣囊衣溶解，过滤后得到碱处理水；
    (3)用酸处理水或者酸调节碱处理水pH至4-7，过滤后得到复合型益生元制剂。
  2. 根据权利要求1中所述的方法，其特征在于，所述柑橘选自柑橘属植物，包括但不限于宽皮柑橘、柚、橙、葡萄柚、柠檬。
  3. 根据权利要求1中所述的方法，其特征在于，所用的酸包括但不限于食品级的盐酸、柠檬酸、草酸、酒石酸、苹果酸、乳酸。
  4. 根据权利要求1中所述的方法，其特征在于，橘瓣和酸溶液的比例为1g:1ml-1g:5ml。
  5. 根据权利要求1中所述的方法，其特征在于，酸溶液浓度为0.4-0.8g/100ml，处理温度为5-80℃，处理时间为20-40min。
  6. 根据权利要求1中所述的方法，其特征在于，所用的碱包括但不限于食品级的NaOH、Na 2CO 3、KOH、K 2CO 3、Mg(OH) 2、Ca(OH) 2。
  7. 根据权利要求1中所述的方法，其特征在于，橘瓣和碱溶液的比例为1g:1ml-1g:5ml。
  8. 根据权利要求1中所述的方法，其特征在于，所用碱溶液浓度为0.4-0.8g/100ml，处理温度为5-80℃，处理时间为10-15min。
  9. 如权利要求1所述方法制备得到的制剂在制备益生元口服液、益生元粉剂、以及逆转抗生素引起的肠道菌群紊乱的保健品中的应用。
  10. 根据权利要求9所述的应用，其特征在于，将柑橘源复合益生元制剂进行喷雾干燥后得到所述柑橘源复合益生元粉剂。
PCT/CN2018/107919 2018-09-27 2018-09-27 一种柑橘源复合益生元制剂的制备方法与应用 WO2020061891A1 (zh)

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Citations (3)

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CN101919522A (zh) * 2010-07-28 2010-12-22 宁波东方九洲食品工贸有限公司 糖水桔子罐头的制备方法
CN103122038A (zh) * 2013-03-05 2013-05-29 浙江大学 一种柑橘罐头生产碱排液提取果胶的工艺
CN106188335A (zh) * 2016-06-29 2016-12-07 高海峰 柑橘罐头加工工艺中同步提取果胶及多酚的方法与系统

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Publication number Priority date Publication date Assignee Title
CN101919522A (zh) * 2010-07-28 2010-12-22 宁波东方九洲食品工贸有限公司 糖水桔子罐头的制备方法
CN103122038A (zh) * 2013-03-05 2013-05-29 浙江大学 一种柑橘罐头生产碱排液提取果胶的工艺
CN106188335A (zh) * 2016-06-29 2016-12-07 高海峰 柑橘罐头加工工艺中同步提取果胶及多酚的方法与系统

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