WO2022165994A1 - 一种广陈皮提取液、制备方法及其应用 - Google Patents

一种广陈皮提取液、制备方法及其应用 Download PDF

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WO2022165994A1
WO2022165994A1 PCT/CN2021/088578 CN2021088578W WO2022165994A1 WO 2022165994 A1 WO2022165994 A1 WO 2022165994A1 CN 2021088578 W CN2021088578 W CN 2021088578W WO 2022165994 A1 WO2022165994 A1 WO 2022165994A1
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tangerine peel
extract
preparation
dipropylene glycol
extraction
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PCT/CN2021/088578
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English (en)
French (fr)
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蔡雪妍
廖思艺
林锐松
黄九九
吴鸿
刘伟
卢敏
是雯菁
Original Assignee
华南农业大学
广州美斛健生物技术有限公司
江门市新会区世纪茗家茶业有限公司
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Publication of WO2022165994A1 publication Critical patent/WO2022165994A1/zh

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    • 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
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00—Drugs for dermatological disorders
    • A61P17/16—Emollients or protectives, e.g. against radiation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00—Drugs for dermatological disorders
    • A61P17/18—Antioxidants, e.g. antiradicals
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • 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
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Definitions

  • the invention relates to the technical field of extraction and processing of effective components of medicinal plants, and is particularly suitable for an extract of tangerine peel, a preparation method and applications thereof.
  • Chenpi is the dry and mature peel of Citrus reticulata Blanco and its cultivars.
  • tangerine peel is divided into tangerine peel and tangerine tangerine peel.
  • Cantonese tangerine peel refers to the dried and ripe peel of Chazhi orange produced in Xinhui District, Jiangmen City, Guangdong province.
  • the main active ingredients contained in tangerine peel are: flavonoids (hesperidin, neohesperidin, tangerine peel, orange peel, etc.), volatile oils, alkaloids, polysaccharides, etc.
  • flavonoids of tangerine peel can not only improve the activity of pepsin, enhance digestive function, but also have good effects on beauty and beauty; hesperidin has excellent anti-ultraviolet damage, anti-oxidation, anti-aging effects, and can be used as sunscreen Effect; tangerine peel has good anti-inflammatory, promotes sebum discharge from sebaceous gland cells, etc., and can relieve skin inflammation such as acne.
  • the polysaccharide components of tangerine peel have the ability to scavenge free radicals, which can achieve anti-oxidation and anti-aging effects.
  • tangerine peel is mainly used in pharmaceutical and health care fields; edible processed products such as tangerine peel candy and tangerine peel beverage are also widely favored by consumers.
  • the extraction technology of effective components of tangerine peel is also becoming more and more mature.
  • microwave-assisted extraction method ultrasonic-assisted extraction method, rapid solvent extraction method (ASE method), high-pressure pulse extraction method and other new methods. Methods are also starting to emerge.
  • the emerging extraction method has the advantages of shortened extraction time and increased extraction rate, and at the same time, combined with column chromatography, the extraction purity can be improved.
  • the emerging method has higher requirements on the instruments used, the extraction environment and the operator in operation, and has the disadvantages of complicated process operation and high equipment cost, and is not suitable for large-scale production. Therefore, the extraction methods commonly used at present do not meet the requirements of large-scale production of cosmetic raw materials.
  • one of the objects of the present invention is to provide a method for preparing a tangerine peel extract with relatively low requirements on production environment and equipment, relatively simple process operation and excellent extraction effect, and the method uses an aqueous solution of dipropylene glycol Double extraction with ethanol solution, compound enzymatic hydrolysis with pectinase and pepsin, and finally mixing and compounding two extracts to obtain the tangerine peel extract.
  • the present invention provides a preparation method of tangerine peel extract, comprising the following steps:
  • Raw material selection and pretreatment use the dried tangerine peel from Xinhui District, Jiangmen City, Guangdong province, aged for 3 years or more, dry in an oven, pulverize with a pulverizer, and sieve to obtain dried tangerine peel powder for use;
  • step (1) dipropylene glycol aqueous solution extraction: the dried tangerine peel powder of step (1) is mixed with the dipropylene glycol aqueous solution in a water bath, filtered, and the filter residue is for subsequent use;
  • Double enzymatic hydrolysis add pectinase and pepsin to the filtrate obtained in step (2) for enzymatic hydrolysis, centrifuge to get the supernatant, and discard the precipitate;
  • step (2) add ethanol solution to the filter residue obtained in step (2), place it in a flash extractor for extraction under room temperature conditions, filter, repeat the extraction of the filter residue once, filter again, and combine the filtrates;
  • step (4) remove ethanol: the filtrate obtained in step (4) is distilled under reduced pressure to remove ethanol, and the concentrated solution is for subsequent use;
  • the oven temperature is 50-70° C.
  • the drying time is 20-40 min
  • the pulverizer is pulverized through a 60-mesh sieve.
  • dried dried tangerine peel at a temperature of 60°C for 30min.
  • step (2) an aqueous solution of dipropylene glycol is used as the extractant to extract, and the specific process of extraction is: taking the dried tangerine peel powder obtained in step (1), adding 100 mL of dipropylene glycol to every 3 g of dried tangerine peel powder.
  • the specific process of enzymatic hydrolysis in step (3) is as follows: adding 0.1-0.3 g/L pectinase and 0.1-0.3 g/L pepsin to the filtrate obtained in step (2), 50-60 g/L After enzymatic hydrolysis at °C for 2-4 hours, and inactivation in 80-degree water bath for 6-10 hours, the supernatant was taken and the precipitate was discarded.
  • the specific process of ethanol extraction in step (4) is as follows: take the filter residue in step (2), add 200 mL of 80% ethanol solution to every 3 g of filter residue, flash for 30min, filter with double-layer filter paper, and repeatedly extract the filter residue Once, soak for 8-12h, filter, and combine the filtrate.
  • step (5) the temperature is maintained at 50-70° C. when the ethanol is removed by distillation under reduced pressure.
  • dipropylene glycol and deionized water are used to dilute the volume to 1000 mL, so that the final concentration of dipropylene glycol is 60%.
  • the second purpose of the present invention is to provide the tangerine tangerine peel extract prepared by the method for preparing the tangerine tangerine peel extract.
  • the third object of the present invention is to provide the application of the said tangerine peel extract in the preparation of cosmetics, and the prepared cosmetics are natural and safe, and have the functions of sun protection, anti-oxidation, anti-aging and the like.
  • the method of the invention adopts dipropylene glycol aqueous solution and ethanol for extraction, combined with the compound enzymatic hydrolysis of pectinase and pepsin, and improves the extraction rate on the premise of not losing or destroying the effective components of tangerine peel as much as possible.
  • the environmental requirements and equipment requirements for the entire extraction process are low, the extraction reagents used are mild and non-toxic to the human body and the environment, and have the advantages of simple operation and high extraction efficiency.
  • the dipropylene glycol solvent used in the extraction process not only has the advantages of enhanced solubility compared with the traditional aqueous solution extraction method, but also is mild and non-toxic to the skin, and even has the effect of water retention and moisturizing.
  • the tangerine peel extract obtained by the invention contains abundant active ingredients such as polysaccharides, hesperidin, and tangerine peel, and the obtained tangerine peel extract is added to cosmetics as a raw material, and has the functions of anti-oxidation, anti-aging, sun protection, whitening and the like. .
  • FIG. 1 is the flow chart of the preparation method of the present invention.
  • the dried tangerine peel described in the embodiment of the present invention is the dried tangerine peel produced in Xinhui District, Jiangmen City, Guangdong province.
  • the pectinase and pepsin described in the examples of the present invention were purchased from Ningxia Heshibi Biotechnology Co., Ltd.
  • Example 1
  • Raw material selection and pre-treatment use tangerine peel aged 3 years, dry in an oven at 60°C for 30 minutes, pulverize with a pulverizer, pass through a 60-mesh sieve, and store in a sealed container for later use.
  • Double enzymatic hydrolysis add 0.1 g/L pectinase and 0.1 g/L pepsin to the filtrate obtained in step (2), enzymatic hydrolysis at 55°C for 3 hours, and water bath at 80°C for 10 hours, take the supernatant and discard the precipitate.
  • Raw material selection and pre-treatment use tangerine peel aged 3 years, dry in an oven at 60°C for 30 minutes, pulverize with a pulverizer, pass through a 60-mesh sieve, and store in a sealed container for later use.
  • Double enzymatic hydrolysis add 0.1 g/L pectinase and 0.2 g/L pepsin to the filtrate, enzymatic hydrolysis at 55°C for 3 hours, and water bath at 80°C for 10 hours, take the supernatant and discard the precipitate.
  • Secondary extraction with ethanol take the filter residue in step (2), add 200 mL of 80% ethanol solution to every 3 g of filter residue, flash for 30 minutes, filter with double-layer filter paper, repeat the extraction of the filter residue once, and soak for 10 hours , filter, and combine the filtrates.
  • Raw material selection and pre-treatment use tangerine peel aged 3 years, dry it in an oven at 60°C for 30 minutes, pulverize with a pulverizer, pass through a 60-mesh sieve, and store it in a sealed container.
  • One-time extraction of dipropylene glycol aqueous solution One-time extraction of dipropylene glycol aqueous solution: take 10 g of dried tangerine peel powder, add 100 mL of an aqueous solution with a dipropylene glycol content of 40% to each 3 g of dried tangerine peel, and water bath at 90°C for 1 h, double-layered Filter with filter paper, and the filter residue is ready for use.
  • Double enzymatic hydrolysis add 0.2 g/L pectinase and 0.1 g/L pepsin to the filtrate, enzymatic hydrolysis at 55°C for 3 hours, and water bath at 80°C for 10 hours, take the supernatant and discard the precipitate.
  • Secondary extraction with ethanol take the filter residue in step (2), add 200 mL of 80% ethanol solution to every 3 g of filter residue, flash for 30 minutes, filter with double-layer filter paper, repeat the extraction of the filter residue once, and soak for 10 hours , filter, and combine the filtrates.

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Abstract

一种广陈皮提取液、制备方法及其应用。所述制备方法为：用双丙甘醇水溶液浸泡提取广陈皮粉后，滤液经果胶酶和胃蛋白酶复合酶解，滤渣经乙醇提取，合并酶解液和醇提液，加双丙甘醇和去离子水，即得广陈皮提取液。该制备方法对生产环境及设备要求较低、工艺操作相对简单且提取效果优良。所得的广陈皮提取液含有丰富的多糖、橙皮苷和川陈皮素等有效成分，作为一种化妆品原料天然安全，具有抗氧化、抗衰老、防晒、美白等功效。

Description

一种广陈皮提取液、制备方法及其应用 技术领域
本发明涉及一种药用植物有效成分提取加工技术领域，尤其适用于一种广陈皮提取液、制备方法及其应用。
背景技术
陈皮是芸香科植物橘(Citrus reticulata Blanco)及其栽培种的干燥成熟果皮，其味苦性辛；具有理气健脾，燥湿化痰的功效。《中国药典》根据产地将陈皮分为陈皮及广陈皮，且自古以广陈皮为上等品。广陈皮专指广东省江门市新会区所产茶枝柑的干燥成熟果皮。陈皮所含主要有效成分有：黄酮类成分(橙皮苷、新橙皮苷、川陈皮素、橘皮素等)、挥发油类成分、生物碱类、多糖等。现代医学发现，陈皮的黄酮类成分不仅可以提高胃蛋白酶活力，增强消化功能，还对美容美颜具有良好的功效；橙皮苷具有优秀的抗紫外损伤、抗氧化、抗衰老功效，可起防晒作用；川陈皮素具有良好的抗炎症、促进皮脂腺细胞的皮脂排出等功效，可舒缓痤疮等皮肤炎症。同时，陈皮的多糖成分具有清除自由基的能力，可达到抗氧化、抗衰老的效果。
目前广陈皮主要应用于制药及保健领域；陈皮糖、陈皮饮料等食用加工品也广受消费者青睐。陈皮有效成分提取技术也日趋成熟，除了传统的煎煮法、乙醇回流法、渗漉法等，微波辅助萃取法、超声辅助萃取法、快速溶剂萃取法(ASE法)、高压脉冲提取法等新方法也开始崭露头角。新兴提取方法相比传统方法具有提取时间减短、提取率增高等优点，同时结合柱色谱法可以提高提取纯度。但是新兴方法 在操作上对使用的仪器、提取的环境以及操作人员具有较高的要求，具有工艺操作复杂、设备成本高等缺点，不适合应用于大规模生产。故目前常用的提取方法均不满足化妆品原料大规模生产的要求。
发明内容
为了解决上述的问题，本发明的目的之一是提供一种对生产环境及设备要求较低、工艺操作相对简单且提取效果优良的广陈皮提取液制备方法，所述方法使用双丙甘醇水溶液和乙醇溶液进行双重提取，以及果胶酶和胃蛋白酶进行复合酶解，最后混合复配两份提取液，从而获得广陈皮提取液。
为了解决上述的问题，本发明提供的技术方案如下：
本发明提供一种广陈皮提取液的制备方法，包括如下步骤：
(1)原料选择与前处理：使用广东省江门市新会区所产，陈化3年及以上的广陈皮，烘箱烘干，粉碎机粉碎，过筛后得到广陈皮粉，备用；
(2)双丙甘醇水溶液提取：步骤(1)的广陈皮粉与双丙甘醇水溶液混合均匀水浴，过滤，滤渣备用；
(3)双酶解：步骤(2)所得滤液中加入果胶酶及胃蛋白酶进行酶解，离心取上清，弃沉淀；
(4)乙醇提取：在步骤(2)所得滤渣中加入乙醇溶液，室温条件下置于闪式提取器中提取，过滤，滤渣重复提取一次，再过滤，合并滤液；
(5)去除乙醇：步骤(4)所得滤液经减压蒸馏，除去乙醇，浓缩液备用；
(6)混合复配：合并步骤(3)所得上清水提液及步骤(5)所得浓缩醇提液，加入双丙甘醇和去离子水，即得广陈皮提取液。
作为本发明的进一步优化，步骤(1)烘箱温度为50～70℃，烘干时间为20～40min，粉碎机粉碎过60目筛。优选以60℃的温度烘干陈皮30min。
作为本发明的进一步改进，步骤(2)中使用双丙甘醇水溶液为提取剂进行提取，提取的具体过程为：取步骤(1)所得的广陈皮粉，每3g广陈皮粉中加100mL双丙甘醇质量含量为20～40％的水溶液，混合均匀，60～90℃水浴1～3h，使用双层滤纸过滤，滤渣备用。
作为本发明的进一步改进，步骤(3)酶解的具体过程为：步骤(2)所得滤液中添加0.1～0.3g/L的果胶酶及0.1～0.3g/L的胃蛋白酶，50～60℃酶解2～4h，80℃水浴6～10h灭活后，取上清，弃沉淀。
作为本发明的进一步改进，步骤(4)乙醇提取的具体过程为：取步骤(2)中的滤渣，每3g滤渣中加200mL 80％乙醇溶液，闪提30min，双层滤纸过滤，滤渣重复提取一次，并浸泡8～12h，过滤，合并滤液。
作为本发明的进一步改进，步骤(5)中使用减压蒸馏去除乙醇时温度维持在50～70℃。
作为本发明的进一步改进，步骤(6)中合并水提液及醇提液后，用双丙甘醇与去离子水定容至1000mL，使双丙甘醇终浓度为60％。
本发明的目的之二是提供由所述的广陈皮提取液的制备方法制备得到的广陈皮提取液。
本发明的目的之三是提供所述的广陈皮提取液在制备化妆品中的应用，制备成的化妆品具有天然安全、具有防晒、抗氧化、抗衰老等功效。
本发明公开了以下技术效果：
本发明所述方法采用双丙甘醇水溶液和乙醇两种溶剂提取，结合果胶酶和胃蛋白酶的复合酶解，在尽可能不损失、破坏广陈皮有效成分的前提下，提高其提取率。整个提取过程所需环境要求及设备要求低，所使用提取试剂对人体及环境温和无毒，且具有操作简单、提取效率高等优点。提取过程中使用的双丙甘醇溶剂，不仅相比于传统水溶液提取法具有溶解性增强的优点，而且对皮肤温和无毒性，甚至具有保水保湿功效。本发明所得广陈皮提取液含有丰富的多糖、橙皮苷和川陈皮素等有效成分，含有获得的广陈皮提取液作为原料液添加到化妆品中，具有抗氧化、抗衰老、防晒、美白等功效。
附图说明
[根据细则91更正 19.05.2021]　
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来 讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为本发明所述制备方法的流程图。
具体实施方式
现详细说明本发明的多种示例性实施方式，该详细说明不应认为是对本发明的限制，而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。
应理解本发明中所述的术语仅仅是为描述特别的实施方式，并非用于限制本发明。另外，对于本发明中的数值范围，应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。
除非另有说明，否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料，但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。本说明书中提到的所有文献通过引用并入，用以公开和描述与所述文献相关的方法和/或材料。在与任何并入的文献冲突时，以本说明书的内容为准。
在不背离本发明的范围或精神的情况下，可对本发明说明书的具体实施方式做多种改进和变化，这对本领域技术人员而言是显而易见的。由本发明的说明书得到的其他实施方式对技术人员而言是显而易见得的。本申请说明书和实施例仅是示例性的。
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等，均为开放性的用语，即意指包含但不限于。
本发明实施例所述广陈皮为广东省江门市新会区所产的广陈皮。本发明实施例所述的果胶酶、胃蛋白酶购自于宁夏和氏璧生物技术有限公司。实施例1
(1)原料选择与前处理：使用陈化3年的广陈皮，用烘箱60℃，30min，烘干，粉碎机粉碎，过60目筛，密封存放备用。
(2)双丙甘醇水溶液一次提取：取10g广陈皮粉，每3g广陈皮粉中加100mL双丙甘醇含量为20％的水溶液，60℃水浴3h，双层滤纸过滤，滤渣备用。
(3)双酶解：步骤所得(2)滤液中添加0.1g/L果胶酶及0.1g/L胃蛋白酶，55℃，酶解3h，80℃水浴10h，取上清，弃沉淀。
(4)乙醇二次提取：取步骤(2)中的滤渣，每3g滤渣中加200mL80％乙醇溶液，闪提30min，双层滤纸过滤，滤渣重复提取一次，并浸泡10h，过滤，合并滤液。
(5)去除乙醇：滤液经70℃减压蒸馏，彻底除去乙醇，浓缩液备用。
(6)混合复配：合并水提液及醇提液后，用双丙甘醇与去离子水定容至1000mL，使其双丙甘醇终浓度为60％。实施例2
(1)原料选择与前处理：使用陈化3年的广陈皮，用烘箱60℃，30min，烘干，粉碎机粉碎，过60目筛，密封存放备用。
(2)双丙甘醇水溶液一次提取：取10g广陈皮粉，每3g广陈皮粉中加100mL双丙甘醇含量为30％的水溶液，80℃水浴2h，双层滤纸过滤，滤渣备用。
(3)双酶解：滤液加入0.1g/L果胶酶及0.2g/L胃蛋白酶，55℃，酶解3h，80℃水浴10h，取上清，弃沉淀。
(4)乙醇二次提取：乙醇二次提取：取步骤(2)中的滤渣，每3g滤渣中加200mL 80％乙醇溶液，闪提30min，双层滤纸过滤，滤渣重复提取一次，并浸泡10h，过滤，合并滤液。
(5)去除乙醇：滤液经70℃减压蒸馏，彻底除去乙醇，浓缩液备用。
(6)混合复配：合并水提液及醇提液后，用双丙甘醇与去离子水定容至1000mL，使其双丙甘醇终浓度为60％。实施例3
(1)原料选择与前处理：使用陈化3年的广陈皮，用烘箱60℃，30min，烘干，粉碎机粉碎，过60目筛，密封存放用。
(2)双丙甘醇水溶液一次提取：双丙甘醇水溶液一次提取：取10g广陈皮粉，每3g广粉中加100mL双丙甘醇含量为40％的水溶液，90℃水浴1h，双层滤纸过滤，滤渣备用。
(3)双酶解：滤液加入0.2g/L果胶酶及0.1g/L胃蛋白酶，55℃，酶解3h，80℃水浴10h，取上清，弃沉淀。
(4)乙醇二次提取：乙醇二次提取：取步骤(2)中的滤渣，每3g滤渣中加200mL 80％乙醇溶液，闪提30min，双层滤纸过滤，滤渣重复提取一次，并浸泡10h，过滤，合并滤液。
(5)去除乙醇：滤液经70℃减压蒸馏，彻底除去乙醇，浓缩液备用。
(6)混合复配：合并水提液及醇提液后，用双丙甘醇与去离子水定容至1000mL，使其双丙甘醇终浓度为60％。
通过多糖、总黄酮、黄酮类物质橙皮苷及川陈皮素含量的测定(表1)，体现所得提取液各类成分的提取率维持在较高水平。通过防晒指数(表2)、总抗氧化能力(表3)、酪氨酸抑制率(表4)的测定，分别体现所得提取液的防晒、抗氧化、抗衰老、美白功效。
表1陈皮提取液的有效成分含量
Figure PCTCN2021088578-appb-000001
表2陈皮提取液防晒指数测定结果
Figure PCTCN2021088578-appb-000002
Figure PCTCN2021088578-appb-000003
表3陈皮提取液总抗氧化能力测定结果
Figure PCTCN2021088578-appb-000004
表4陈皮提取液的酪氨酸抑制率
Figure PCTCN2021088578-appb-000005
表2的结果表明稀释5、10倍的陈皮提取液具有良好的防晒功效；表3的结果表明稀释5、10、50倍的陈皮提取液具有明显的抗氧化功效；表4的结果表明稀释10、50倍的陈皮提取液具有优秀的美白功效。
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。

Claims (9)

  1. 一种广陈皮提取液的制备方法，其特征在于，包括以下步骤：
    (1)原料选择与前处理：使用陈化3年及以上的广陈皮，烘干，粉碎，过筛后得到广陈皮粉，备用；
    (2)双丙甘醇水溶液提取：所述广陈皮粉与双丙甘醇水溶液混合均匀水浴，过滤，滤渣备用；
    (3)双酶解：步骤(2)所得滤液中加入果胶酶及胃蛋白酶进行酶解，离心取上清，弃沉淀；
    (4)乙醇提取：在步骤(2)所得滤渣中加入乙醇溶液，室温条件下，进行提取，过滤，滤渣重复提取一次，再过滤，合并滤液；
    (5)去除乙醇：步骤(4)所得滤液经减压蒸馏，除去乙醇，浓缩液备用；
    (6)混合复配：合并步骤(3)所得上清水提液及步骤(5)所得浓缩醇提液，加入双丙甘醇和去离子水，即得广陈皮提取液。
  2. 根据权利要求1所述的一种广陈皮提取液的制备方法，其特征在于，步骤(1)烘干温度为50～70℃，烘干时间为20～40min，粉碎机粉碎过筛。
  3. 根据权利要求1所述的一种广陈皮提取液制备方法，其特征在于，步骤(2)中使用双丙甘醇水溶液为提取剂进行提取，提取的具体过程为：取步骤(1)所得的广陈皮粉，每3g广陈皮粉中加100mL双丙甘醇质量含量为20～40％的水溶液，混合均匀，60～90℃水浴1～3h，使用双层滤纸过滤，滤渣备用。
  4. 根据权利要求1所述的一种广陈皮提取液制备方法，其特征在于，步骤(3)使用果胶酶及胃蛋白酶进行复合酶解，酶解的具体过程为：步骤(2)所得滤液中添加0.1～0.3g/L的果胶酶及0.1～0.3g/L胃蛋白酶，50～60℃酶解2～4h，80℃水浴6～10h灭活后，取上清，弃沉淀。
  5. 根据权利要求1所述的一种广陈皮提取液的制备方法，其特征在于，步骤(4)乙醇提取的具体过程为：取步骤(2)中的滤渣，每3g滤渣中加200mL 80％乙醇溶液，闪提30min，双层滤纸过滤，滤渣重复提取一次，并浸泡8～12h，过滤，合并滤液。
  6. 根据权利要求1所述的一种广陈皮提取液制备方法，其特征在于，步骤(5)中使用减压蒸馏去除乙醇时温度维持在50～70℃。
  7. 根据权利要求1所述的一种广陈皮提取液制备方法，其特征在于，步骤(6)中合并水提液及醇提液后，用双丙甘醇与去离子水定容至1000mL，使双丙甘醇终浓度为60％。
  8. 一种广陈皮提取液，其特征在于，根据权利要求1～7任一项所述的广陈皮提取液的制备方法制备得到。
  9. 一种根据权利要求8所述的广陈皮提取液在制备化妆品中的应用。
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