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CN103845343A - Application of pecan sterol extractive in preparation of anti-inflammatory materials - Google Patents

Application of pecan sterol extractive in preparation of anti-inflammatory materials Download PDF

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CN103845343A
CN103845343A CN201410079250.9A CN201410079250A CN103845343A CN 103845343 A CN103845343 A CN 103845343A CN 201410079250 A CN201410079250 A CN 201410079250A CN 103845343 A CN103845343 A CN 103845343A
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pecan
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CN103845343B (en
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陆柏益
周菲
杨佳佳
胡银洲
毛淑琴
蒋易蓉
洪雅雯
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Zhejiang University ZJU
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Abstract

本发明公开了一种山核桃甾醇提取物在制备消炎物品中的应用;该消炎物品包括消炎药、用于消炎的日用化妆品、或用于消炎的保健品。山核桃甾醇提取物中总甾醇重量含量为10~50%,并且所述的总甾醇包括β-谷甾醇、岩皂甾醇、菜油甾醇和豆甾醇。总甾醇中β-谷甾醇的重量含量为70-95%,并且β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比为70~95:1~10:2~12:1~15。

The invention discloses the application of hickory nut sterol extract in preparing anti-inflammatory articles; the anti-inflammatory articles include anti-inflammatory drugs, daily cosmetics for anti-inflammation, or health products for anti-inflammation. The weight content of the total sterols in the hickory nut sterol extract is 10-50%, and the total sterols include β-sitosterol, rock soap sterol, campesterol and stigmasterol. The weight content of β-sitosterol in the total sterols is 70-95%, and the weight ratio between β-sitosterol, rock saponosterol, campesterol and stigmasterol is 70-95:1-10:2-12:1 ~15.

Description

山核桃甾醇提取物在制备消炎物品中的应用Application of hickory nut sterol extract in preparation of anti-inflammatory articles

技术领域technical field

本发明涉及农副产品深加工及综合利用领域。更具体地涉及一种从山核桃中提取的植物甾醇类提取物的用途。The invention relates to the field of deep processing and comprehensive utilization of agricultural and sideline products. More specifically, it relates to the use of a phytosterol extract extracted from hickory nuts.

背景技术Background technique

山核桃(Carya)又名“小胡桃”、核桃楸,系国家3级保护的濒危植物。属胡桃科、胡桃属植物,起源于第三纪及白垩纪,是被子植物中较古老的类群之一。山核桃生长在气候优越、土壤肥沃、植被茂盛的自然环境中,属纯野生果类,是集山地之灵气哺育而成,无任何公害污染的天然绿色食品。山核桃属种类较多,约有30种,主产美洲,我国有临安山核桃、大别山山核桃、湖南山核桃、贵州山核桃和云南山核桃5种,另从美洲引入栽培美国山核桃。山核桃属中种植量较大的为美国山核桃和临安山核桃。美国山核桃年产量为78000吨-18000吨,市场价值可达200亿到400亿美元。临安山核桃主产于浙、皖交界的天目山区,临安是浙江山核桃主产地之一。截至2011年,杭州市山核桃种植面积超过80万亩,产值超过23亿元。Hickory (Carya), also known as "small walnut" and walnut catalpa, is an endangered plant under national third-level protection. Juglandaceae, Juglans, originated in the Tertiary and Cretaceous, is one of the older groups of angiosperms. Hickory nuts grow in a natural environment with superior climate, fertile soil and lush vegetation. It is a pure wild fruit and is a natural green food without any pollution pollution. There are many types of hickory, about 30 species, mainly produced in America. In my country, there are 5 species of hickory in Lin'an, Dabie Mountain, Hunan, Guizhou and Yunnan. In addition, American hickory is introduced and cultivated from America. Among the hickory genus, American hickory and Lin'an hickory are the most planted. The annual output of American pecans is 78,000-18,000 tons, and the market value can reach 20 billion to 40 billion US dollars. Lin'an hickory is mainly produced in the Tianmu Mountains at the junction of Zhejiang and Anhui. Lin'an is one of the main producing areas of hickory in Zhejiang. As of 2011, the hickory planting area in Hangzhou City exceeded 800,000 mu, and the output value exceeded 2.3 billion yuan.

山核桃中天然活性成分种类较多,除基本的营养成分外,山核桃中含有的主要功能性成分有:酚酸、黄酮、甾体类、萜类、生物碱、活性多糖、维生素等,其中以酚酸、生育酚、甾醇等为主。目前对山核桃活性成分的研究多局限在具有本国资源特色的山核桃品种上,有其是美国山核桃的研究较为全面和深入。There are many types of natural active ingredients in pecans. In addition to basic nutrients, the main functional ingredients contained in pecans are: phenolic acids, flavonoids, steroids, terpenes, alkaloids, active polysaccharides, vitamins, etc., among which Mainly phenolic acids, tocopherols, sterols, etc. At present, the research on the active ingredients of pecans is mostly limited to the pecan varieties with the characteristics of domestic resources, especially the research on American pecans is more comprehensive and in-depth.

中国是山核桃生产、利用和研究的古国。然而国内科研工作者对山核桃资源的深入开发和利用上仍处于探索阶段,如利用山核桃制备膳食纤维、分离活性蛋白、多糖,开发高营养的饲料等。China is an ancient country of hickory production, utilization and research. However, the further development and utilization of pecan resources by domestic scientific researchers are still in the exploratory stage, such as using pecans to prepare dietary fiber, separating active proteins and polysaccharides, and developing high-nutrition feed.

Laura等(2010)研究山核桃中酚酸含量极为丰富,主要含有鞣花酸、没食子酸、绿原酸、对羟基苯甲酸,其中鞣花酸为其主要成分。Margit等(2006)系统研究了10种常见坚果中的生育酚种类和含量,研究表明美国山核桃生育酚以γ-生育酚为主,其含量可达生育酚总量的90%以上。Laura et al. (2010) studied that pecans are extremely rich in phenolic acids, mainly containing ellagic acid, gallic acid, chlorogenic acid, and p-hydroxybenzoic acid, of which ellagic acid is the main component. Margit et al. (2006) systematically studied the types and contents of tocopherols in 10 common nuts. The research showed that the tocopherols of American hickory nuts are mainly γ-tocopherols, and their content can reach more than 90% of the total tocopherols.

然而,迄今为止人们多山核桃中的许多构成成分和功能还了解较少。为了更有效地开发和利用山核桃资源,本领域迫切需要发现和开发山核桃中具有有益功能的各种成分。However, so far, many constituents and functions of hickory nuts are still poorly understood. In order to develop and utilize hickory nut resources more effectively, it is urgent to discover and develop various components with beneficial functions in hickory nut.

植物甾醇是3位为羟基的甾体化合物,以环戊烷全氢菲为主体骨架,天然植物甾醇种类繁多,主要包括β-谷甾醇、豆甾醇、菜籽甾醇和菜油甾醇四种无甲基甾醇。一般认为,植物油及其加工产品是植物甾醇最丰富的天然来源,其次是谷物副产品和坚果。玉米油、菜籽油、米糠油、小麦胚芽油、黑麦、小麦、大麦和燕麦都含有丰富的甾醇。关于植物甾醇的应用,迄今已发表了大量的著作,领域涉及医药、化妆品、食品、饲料、光学产品、油漆、颜料、树脂、造纸、纺织、杀虫剂及除草剂等。以植物甾醇为原料,可合成几乎所有的甾体药物,其在世界范围内是一个有着40亿美元的产业。因此,植物甾醇的分离和纯化得到了人们的高度重视。Phytosterol is a steroidal compound with a hydroxyl group in the 3 position, with cyclopentane perhydrophenanthrene as the main skeleton. There are many kinds of natural phytosterols, mainly including β-sitosterol, stigmasterol, brassicasterol and campesterol. Sterol. It is generally believed that vegetable oil and its processed products are the most abundant natural sources of phytosterols, followed by grain by-products and nuts. Corn oil, canola oil, rice bran oil, wheat germ oil, rye, wheat, barley and oats are all rich in sterols. Regarding the application of phytosterols, a large number of works have been published so far, covering the fields of medicine, cosmetics, food, feed, optical products, paints, pigments, resins, papermaking, textiles, insecticides and herbicides. Using phytosterols as raw materials, almost all steroid drugs can be synthesized, which is an industry with 4 billion US dollars worldwide. Therefore, the separation and purification of phytosterols have been highly valued.

植物油精炼副产物,制糖副产物以及造纸废液中都具有丰富的甾醇。其中,植物油精炼副产物是甾醇的主要来源。从原料中提取甾醇通常分两步进行。先从原料中提取粗甾醇,然后再进一步精制。常用方法包括溶剂结晶法、分子蒸馏法、酶法、干式皂化法和络合法。但这些工艺均还不够理想,或是耗费大量易燃有机溶剂,或是产品纯度不高,或是高温易使甾醇分解。Vegetable oil refining by-products, sugar by-products and papermaking waste liquids are rich in sterols. Among them, the by-products of vegetable oil refining are the main source of sterols. Extraction of sterols from raw materials is usually carried out in two steps. Crude sterols are first extracted from raw materials and then further refined. Common methods include solvent crystallization, molecular distillation, enzymatic, dry saponification, and complexation. But these processes are not ideal enough, or consume a large amount of flammable organic solvents, or the product purity is not high, or high temperature easily decomposes sterols.

目前现有的山核桃提取物,其总甾醇仅包含β-谷甾醇和豆甾醇。At present, the total sterols of pecan extracts currently available only contain β-sitosterol and stigmasterol.

发明内容Contents of the invention

本发明要解决的技术问题是提供一种从山核桃中提取的植物甾醇类提取物--山核桃甾醇提取物的用途。The technical problem to be solved by the present invention is to provide a phytosterol extract extracted from hickory nuts - the use of hickory nut sterol extract.

为了解决上述技术问题,本发明提供山核桃甾醇提取物在制备消炎物品中的应用。该消炎物品包括消炎药、用于消炎的日用化妆品、或用于消炎的保健品。In order to solve the above technical problems, the present invention provides the application of hickory nut sterol extract in the preparation of anti-inflammatory articles. The anti-inflammatory articles include anti-inflammatory drugs, daily cosmetics for anti-inflammation, or health products for anti-inflammation.

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的改进:所述山核桃甾醇提取物中总甾醇重量含量为10~50%,并且所述的总甾醇包括β-谷甾醇、岩皂甾醇、菜油甾醇和豆甾醇(基本由上述4种甾醇组成)。As an improvement in the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the total sterol weight content in the pecan sterol extract is 10 to 50%, and the total sterols include β-sitosterol, rock Saponasterol, campesterol and stigmasterol (consisting basically of the above 4 sterols).

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:总甾醇中β-谷甾醇的重量含量为70-95%,并且β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比为70~95:1~10:2~12:1~15。As a further improvement of the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the weight content of β-sitosterol in the total sterols is 70-95%, and β-sitosterol, rock soap sterol, campesterol, soybean The weight ratio between sterols is 70-95:1-10:2-12:1-15.

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:该提取物中总甾醇重量含量为20-40%,并且总甾醇中β-谷甾醇的重量含量为75-90%。As a further improvement of the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the weight content of total sterols in the extract is 20-40%, and the weight content of β-sitosterol in the total sterols is 75-90% .

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比为75~90:2~10:2~10:2~11。As a further improvement of the application of the hickory nut sterol extract of the present invention in the preparation of anti-inflammatory articles: the weight ratio between β-sitosterol, rock saponosterol, campesterol and stigmasterol is 75~90:2~10:2~ 10:2-11.

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比例为76.5:9.6:2.9:11。As a further improvement of the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the weight ratio between β-sitosterol, rock saponosterol, campesterol and stigmasterol is 76.5:9.6:2.9:11.

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:山核桃甾醇提取物的制备方法包括以下步骤:As a further improvement of the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the preparation method of the pecan sterol extract comprises the following steps:

1)、将山核桃粉碎(20-40目)后作为原料(含水量约5~10%,重量%),在分离釜中,于下述条件对原料进行超临界流体萃取:萃取剂为CO2,萃取压力为15~35MPa,萃取温度为40~70℃,分离温度为30~50℃,分离压力为4~8MPa,循环动态萃取1~5h;1) Grinding hickory nuts (20-40 mesh) as raw material (water content about 5-10%, weight%), in the separation kettle, the raw material is subjected to supercritical fluid extraction under the following conditions: the extraction agent is CO 2. The extraction pressure is 15-35MPa, the extraction temperature is 40-70°C, the separation temperature is 30-50°C, the separation pressure is 4-8MPa, and the cycle dynamic extraction is 1-5h;

2)、从分离釜中取出萃取物,经干燥(于50~60℃干燥40~60分钟),从而获得山核桃甾醇提取物。2) Take out the extract from the separation kettle and dry it (at 50-60°C for 40-60 minutes), so as to obtain the hickory nut sterol extract.

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:步骤1)中的萃取压力为20~30MP,萃取温度为45~65℃,使用夹带剂,所述夹带剂的用量为山核桃重量的5~15%;所述夹带剂为C1~C4的醇类有机溶剂(即,C1~C4的醇类有机溶剂中的任意一种)或C1~C4的酮类有机溶剂(即,C1~C4的酮类有机溶剂中的任意一种)。As a further improvement of the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the extraction pressure in step 1) is 20-30MP, the extraction temperature is 45-65°C, an entrainer is used, and the amount of the entrainer is 5% to 15% of the weight of hickory; the entrainer is a C1-C4 alcohol organic solvent (that is, any one of the C1-C4 alcohol organic solvent) or a C1-C4 ketone organic solvent ( That is, any one of C1-C4 ketone organic solvents).

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:将山核桃甾醇提取物制备成组合物,所述组合物由0.01-99.9wt%的山核桃甾醇提取物和作为余量的可接受载体组成。As a further improvement of the application of the Cargo sterol extract of the present invention in the preparation of anti-inflammatory articles: the Cargo sterol extract is prepared into a composition, and the composition is composed of 0.01-99.9wt% Cargo sterol extract and the remaining amount of acceptable carrier composition.

作为本发明的山核桃甾醇提取物在制备消炎物品中的应用的进一步改进:所述组合物为药物组合物、保健品组合物、食品组合物或化妆品组合物。As a further improvement of the application of the pecan sterol extract of the present invention in the preparation of anti-inflammatory articles: the composition is a pharmaceutical composition, a health product composition, a food composition or a cosmetic composition.

本发明人经过多年深入研究,对山核桃的各种成分进行了提取分离,获得了一种可有效消炎的提取物,对该提取物的研究表明,该提取物主要含β-谷甾醇、岩皂甾醇、菜油甾醇和豆甾醇等成分,在此基础上完成了本发明。After many years of in-depth research, the inventor has extracted and separated various components of hickory nuts, and obtained an extract that can effectively reduce inflammation. The research on the extract shows that the extract mainly contains β-sitosterol, rock Compositions such as soap sterol, campesterol and stigmasterol have completed the present invention on this basis.

如本文所用,山核桃指山核桃树的果实。可用于本发明山核桃可以是山核桃仁,也可以是山核桃皮,也可以是山核桃加工过程中产生的废弃物,如山核桃壳和废果等。优选原料是山核桃壳和山核桃仁。As used herein, hickory refers to the fruit of the hickory tree. The hickory nuts that can be used in the present invention can be hickory kernels, hickory skins, or wastes generated during hickory processing, such as hickory shells and waste fruits. Preferred starting materials are hickory shells and hickory kernels.

本发明采用的原料可以进行预处理,也可以不经过预处理。一种优选原料是粉末形式的山核桃仁。例如,收集山核桃仁、山核桃皮、山核桃壳,打成浆压榨或直接晾晒到一定程度,再干燥到含水量约5~10%,将其粉碎到约20~40目的粉末。The raw materials used in the present invention may or may not be pretreated. A preferred starting material is pecan kernels in powder form. For example, hickory kernels, hickory skins, and hickory shells are collected, pulped, pressed or directly aired to a certain extent, then dried to a water content of about 5-10%, and crushed to about 20-40 mesh powder.

可用于本发明的山核桃品种没有特别限制,可以是不同种的山核桃,优选临安山核桃和美国山核桃。The hickory varieties that can be used in the present invention are not particularly limited, and may be different kinds of hickory, preferably Lin'an hickory and American hickory.

如本文所用,“本发明的活性物质”指山核桃甾醇提取物。As used herein, "active substance of the present invention" refers to pecan sterol extract.

如本文所用,“本发明的活性物质制剂”或“本发明的活性组合物”指含有山核桃甾醇提取物的组合物,包括药物组合物和保健品组合物。As used herein, "the active substance preparation of the present invention" or "the active composition of the present invention" refers to a composition containing the sterol extract of hickory nuts, including a pharmaceutical composition and a health product composition.

本发明的山核桃甾醇提取物宜用超临界流体萃取技术提取,虽然也可其他方法提取。The pecan sterol extract of the present invention is preferably extracted by supercritical fluid extraction technology, although it can also be extracted by other methods.

一种优选的方法是采用超临界流体萃取技术从山核桃及其加工废弃物(山核桃壳)中提取甾醇类化合物。在一优选方式中,萃取剂为CO2,萃取压力为15~35MPa,萃取温度为40~70℃,分离温度为30~50℃,分离压力为4~8MPa,并可以在萃取过程中加入醇或酮作为夹带剂,起到增效作用。A preferred method is to extract sterols from pecans and their processing waste (pecan shells) using supercritical fluid extraction. In a preferred mode, the extractant is CO 2 , the extraction pressure is 15-35MPa, the extraction temperature is 40-70°C, the separation temperature is 30-50°C, the separation pressure is 4-8MPa, and alcohol can be added during the extraction process. Or ketone acts as an entrainer to play a synergistic effect.

在更优选的方式中,将约20-40目山核桃粉末放入超临界萃取釜中,萃取剂选CO2,CO2经压缩机升压同时对萃取釜加温,当萃取压力达到15~35MPa,萃取温度达到40~70℃时,开始循环;在循环过程中,CO2和萃取物在分离器中经减压,将萃取物在分离器中析出,CO2循环使用,分离釜1设定分离压力为6~8MPa、温度为35~45℃,分离釜2设定分离压力为4~7MPa、温度为30~35℃;在萃取过程中使用或不使用夹带剂的状态下,循环动态萃取1~5h,使用的夹带剂可以是C1~C4的醇或酮类有机溶剂(如甲醇、乙醇、丙酮等),用量一般为原料重量的5~15%。萃取完成后,从分离釜中取出萃取物,经低温干燥后,就得到山核桃甾醇提取物,并从分离釜中回收夹带剂(在使用夹带剂的状态下),停机从萃取釜中取出萃余物。In a more preferred way, put about 20-40 mesh hickory powder into the supercritical extraction kettle, the extraction agent is CO 2 , CO 2 is boosted by the compressor and the extraction kettle is heated at the same time, when the extraction pressure reaches 15~ 35MPa, when the extraction temperature reaches 40-70°C, the cycle starts; during the cycle, CO2 and the extract are decompressed in the separator, and the extract is precipitated in the separator, and the CO2 is recycled, and the separation tank 1 is set The separation pressure is set at 6-8MPa, the temperature is 35-45°C, the separation pressure of the separation tank 2 is set at 4-7MPa, and the temperature is 30-35°C; in the state of using or not using an entrainer during the extraction process, the cycle dynamic Extract for 1-5 hours, the entrainer used can be C1-C4 alcohol or ketone organic solvent (such as methanol, ethanol, acetone, etc.), and the dosage is generally 5-15% of the weight of the raw material. After the extraction is completed, take out the extract from the separation kettle, and after drying at low temperature, you can get the pecan sterol extract, and recover the entrainer from the separation kettle (in the state of using the entrainer), stop the machine and take out the extract from the extraction kettle remnants.

本发明的山核桃甾醇提取物是一种以β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇为主的混合物。用Liebermann Burchard分光光度法检测,以β-谷甾醇为标准品,测得提取物中总甾醇的含量为10~50%(较佳地为20~40%);用UPLC技术分析,其中β-谷甾醇含量(相对于总甾醇而言)为70~95%(较佳为75~90%),β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间比例为70~95:1~10:2~12:1~15。更佳地为75~90:2~10:2~10:2~11。The pecan sterol extract of the present invention is a mixture mainly containing β-sitosterol, rockapasterol, campesterol and stigmasterol. Detect with Liebermann Burchard spectrophotometry, take β-sitosterol as standard substance, measure the content of total sterols in the extract to be 10~50% (preferably 20~40%); Analyze with UPLC technique, wherein β- The content of sitosterol (relative to the total sterols) is 70-95% (preferably 75-90%), and the ratio between β-sitosterol, rock saponosterol, campesterol and stigmasterol is 70-95:1~ 10:2~12:1~15. More preferably, it is 75-90:2-10:2-10:2-11.

本发明的山核桃甾醇提取物具有消炎等有益作用,因此可用于制备用于消炎的药物、日用化妆品、保健品。因此,本发明还提供了一种含有本发明的山核桃甾醇提取物作为有效成份的组合物(包括药物组合物、保健品组合物、食品组合物和化妆品组合物等)。这些组合物可用于预防、治疗或辅助治疗炎症。The hickory nut sterol extract of the invention has beneficial effects such as anti-inflammation, so it can be used to prepare anti-inflammatory medicines, daily cosmetics and health care products. Therefore, the present invention also provides a composition (including pharmaceutical composition, health product composition, food composition and cosmetic composition, etc.) containing the hickory nut sterol extract of the present invention as an active ingredient. These compositions can be used to prevent, treat or assist in the treatment of inflammation.

在获得山核桃甾醇提取物后,可用常规方法将其与药学上、食品学上或保健品或化妆品上可接受的载体、赋形剂或稀释剂相混合,形成本发明的药物组合物、食品组合物、保健品组合物或化妆品组合物。这类载体包括(但并不限于):盐水、缓冲液、葡萄糖、水、甘油、乙醇、及其组合。After obtaining the pecan sterol extract, it can be mixed with pharmaceutically, food science, health care products or cosmetically acceptable carriers, excipients or diluents by conventional methods to form the pharmaceutical composition of the present invention, food Composition, health product composition or cosmetic composition. Such carriers include, but are not limited to: saline, buffer, dextrose, water, glycerol, ethanol, and combinations thereof.

以药物组合物或保健品组合物为例,它们可以为固态(如颗粒剂、片剂、冻干粉、栓剂、胶囊、舌下含片)或液态(如口服液)或其他合适的形状。本发明的活性成分(山核桃甾醇提取物))的含量通常为组合物重量的0.01-99.9%,较佳地为1-99%,更较佳地为2-95%,进一步更佳地为5-90%,最佳地10-80%。Taking pharmaceutical compositions or health product compositions as an example, they can be in solid state (such as granules, tablets, freeze-dried powder, suppositories, capsules, sublingual tablets) or liquid state (such as oral liquid) or other suitable shapes. The content of the active ingredient of the present invention (Pecanus sterol extract)) is usually 0.01-99.9% of the weight of the composition, preferably 1-99%, more preferably 2-95%, and even more preferably 5-90%, optimally 10-80%.

药物组合物可以为单剂或多剂形式。按施用剂量计,通常含有10-2000mg/剂,较佳地约20-1000mg/剂,更佳地50-500mg/剂。The pharmaceutical compositions may be in single or multiple dose form. According to the administration dose, it usually contains 10-2000 mg/dose, preferably about 20-1000 mg/dose, more preferably 50-500 mg/dose.

本发明的药物组合物可以通过常规途径进行给药,优选方式是口服。药物制剂应与给药方式相匹配。本发明药物的施用量,按山核桃甾醇提取物计算,通常为每天约0.1-500mg/kg体重,较佳地约0.5-50mg/kg体重。此外,本发明的制剂还可与其他治疗剂一起使用,例如,其他治疗剂包括各种现有的消炎药。The pharmaceutical composition of the present invention can be administered through conventional routes, preferably orally. The pharmaceutical formulation should match the mode of administration. The dosage of the medicament of the present invention is usually about 0.1-500 mg/kg body weight per day, preferably about 0.5-50 mg/kg body weight, calculated on the basis of the hickory nut sterol extract. In addition, the formulations of the present invention can also be used with other therapeutic agents, including, for example, various existing anti-inflammatory drugs.

本发明的主要优点是:The main advantages of the present invention are:

(a)提供了一种来源广阔、组成明晰、品质优良、质量可控、用途广泛并具有多种生理和药理活性的山核桃甾醇提取物。(a) Provide a pecan sterol extract with broad sources, clear composition, high quality, controllable quality, wide application and various physiological and pharmacological activities.

(b)通过超临界CO2流体萃取技术实现了山核桃及其加工废弃物中植物甾醇的高效提取,并且工艺操作简便,得到的山核桃甾醇提取物质量好,品质稳定。(b) The high-efficiency extraction of phytosterols in pecans and their processing wastes was realized by supercritical CO 2 fluid extraction technology, and the process was easy to operate, and the obtained sterol extracts of pecans were of good and stable quality.

(c)、山核桃甾醇提取物具有消炎的性能。(c) Pecan sterol extract has anti-inflammatory properties.

附图说明Description of drawings

下面结合附图对本发明的具体实施方式作进一步详细说明。The specific implementation manners of the present invention will be described in further detail below in conjunction with the accompanying drawings.

图1为山核桃甾醇提取物的超高效液相色谱图;Fig. 1 is the ultra high performance liquid phase chromatogram of Carya sterol extract;

图2山核桃甾醇提取物中植物甾醇的结构图。Figure 2 Structural diagram of phytosterols in pecan sterol extract.

具体实施方式Detailed ways

下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。下列实施例中未注明具体条件的实验方法,通常按照常规条件,或按照制造厂商所建议的条件。Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. For the experimental methods without specific conditions indicated in the following examples, the conventional conditions or the conditions suggested by the manufacturer are usually followed.

通用方法general method

1)山核桃甾醇提取物中植物甾醇含量测定——Liebermann Burchard比色法1) Determination of phytosterol content in pecan sterol extract——Liebermann Burchard colorimetric method

将样品用三氯甲烷萃取溶解后取下层三氯甲烷层。准确移取1ml三氯甲烷样品溶液,加入醋酐2ml和浓硫酸1滴,振荡摇匀后用1cm的比色杯在625nm波长处测定吸光值。每一个样品平行测定2次,以β-谷甾醇为标准品,根据标准曲线换算成相应的总甾醇含量,取平均值得到样品中植物总甾醇的含量。After the sample was extracted and dissolved with chloroform, the lower chloroform layer was removed. Accurately pipette 1ml of chloroform sample solution, add 2ml of acetic anhydride and 1 drop of concentrated sulfuric acid, shake well and measure the absorbance at 625nm wavelength with a 1cm cuvette. Each sample was measured twice in parallel, using β-sitosterol as a standard, converted to the corresponding total sterol content according to the standard curve, and taking the average value to obtain the total phytosterol content in the sample.

2)山核桃甾醇提取物的有效成分分析——超高效液相色谱(UPLC)2) Analysis of active components of pecan sterol extract——Ultra Performance Liquid Chromatography (UPLC)

通过使用超高效液相色谱分析萃取物中存在的甾醇成分和含量。The sterol composition and content present in the extract were analyzed by using ultra-high performance liquid chromatography.

UPLC条件:Waters公司的超高效液相色谱,ACQUITY BEH C18色谱柱(2.1mm i.d.*150mm,1.7μm,Waters),流动相为乙腈:水=9:1,流速为0.6mL/min,柱温为40℃,检测波长为210nm。检测扫面范围为210nm至400nm。UPLC conditions: ultra-high performance liquid chromatography from Waters, ACQUITY BEH C18 column (2.1mm i.d.*150mm, 1.7μm, Waters), mobile phase is acetonitrile: water = 9:1, flow rate is 0.6mL/min, column temperature The temperature is 40°C, and the detection wavelength is 210nm. The detection scan range is from 210nm to 400nm.

以下实施例中所选用的超临界萃取仪为常规的一萃二分CO2循环式,包括萃取釜、分离釜、CO2储罐、夹带剂泵等。The supercritical extraction apparatus selected in the following examples is a conventional one-extraction-two-partition CO2 circulation type, including an extraction tank, a separation tank, a CO2 storage tank, an entrainer pump, and the like.

实施例1、一种山核桃甾醇提取物的制备方法:Embodiment 1, a kind of preparation method of pecan sterol extract:

将临安山核桃剥壳后,将山核桃仁打成浆,初步晒干后,再用微波干燥到水分含量为5%(重量%),粉碎成20目的山核桃粉末5kg作为原料,并将其放入超临界萃取釜中,升温到50℃,开动柱塞泵泵入CO2,通过预热器进入萃取釜中,当压力达到25MPa,开始循环;开启夹带剂泵,使10%原料重量的乙醇通过预热器后同时进入萃取釜;在循环过程中,CO2和萃取物在分离器中经减压,将萃取物在分离器中析出,CO2循环使用,分离釜1设定分离压力为8MPa、温度为40℃,分离釜2设定分离压力为5MPa、温度为30℃;萃取4h后,从分离釜1、2中取出萃取物60g,得率为1.2%,经低温干燥(即,于50-60℃干燥50分钟)后,得到45g的山核桃甾醇提取物,并从分离釜1、2中回收夹带剂;停机从萃取釜中取出萃余物。After shelling the Linan hickory nuts, beat the hickory nut kernels into pulp, dry them in the sun, dry them with microwave until the moisture content is 5% (weight %), crush them into 5kg of 20-mesh hickory nut powder as raw material, and make them Put it into a supercritical extraction kettle, raise the temperature to 50°C, start the plunger pump to pump CO 2 into the extraction kettle through the preheater, and start circulation when the pressure reaches 25MPa; turn on the entrainer pump to make 10% of the raw material weight Ethanol enters the extraction tank after passing through the preheater; during the circulation process, CO2 and the extract are decompressed in the separator, and the extract is precipitated in the separator, CO2 is recycled, and the separation pressure is set in the separation tank 1 8MPa, temperature 40°C, separation tank 2 set separation pressure to 5MPa, temperature 30°C; after extraction for 4 hours, take out 60g of extract from separation tank 1 and 2, the yield is 1.2%, after low temperature drying (i.e. , after drying at 50-60°C for 50 minutes), 45g of pecan sterol extract was obtained, and the entrainer was recovered from the separation tank 1 and 2; the extraction tank was shut down to take out the raffinate.

对提取物进行成分分析,结果如图1-2所示。The extract was analyzed for its components, and the results are shown in Figure 1-2.

图1表明山核桃甾醇提取物成分包括:9min左右为岩皂甾醇,11min左右为菜油甾醇,12min左右为豆甾醇,16min左右为β-谷甾醇。Figure 1 shows that the components of the hickory nut sterol extract include: about 9 minutes is fusapesterol, about 11 minutes is campesterol, about 12 minutes is stigmasterol, and about 16 minutes is β-sitosterol.

图2证实了提取物中含有岩皂甾醇(fucosterol)、菜油甾醇(campesterol)、豆甾醇(stigmasterol)、β-谷甾醇(β-sitosterol)。Figure 2 confirms that the extract contains fucosterol, campesterol, stigmasterol, and β-sitosterol.

UPLC法分析山核桃甾醇提取物的成分含量,其总甾醇含量为25.6%,β-谷甾醇为19.6%(即,总甾醇中β-谷甾醇的含量为76.56%),β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比例为76.5:9.6:2.9:11。The UPLC method analyzes the component content of pecan sterol extract, and its total sterol content is 25.6%, and β-sitosterol is 19.6% (that is, the content of β-sitosterol in total sterol is 76.56%), β-sitosterol, rock The weight ratio among saponasterol, campesterol and stigmasterol is 76.5:9.6:2.9:11.

实施例2、一种山核桃甾醇提取物的制备方法:Embodiment 2, a kind of preparation method of pecan sterol extract:

将美国山核桃壳壳初步晒干后用热风(70~90℃)干燥到水分含量为5%,粉碎成20目的山核桃壳粉末5kg作为原料,并将其放入超临界萃取釜中,升温到60℃,开动柱塞泵泵入CO2,通过预热器进入萃取釜中,当压力达到30MPa,开始循环;开启夹带剂泵,使10%的丙酮通过预热器后同时进入萃取釜;在循环过程中,CO2和萃取物在分离器中经减压,将萃取物在分离器中析出,CO2循环使用,分离釜1设定分离压力为8MPa、温度为45℃,分离釜2设定分离压力为5MPa、温度为30℃;萃取2.5h后,从分离釜1、2中取出萃取物35g,得率为0.7%,经低温干燥后,得到31g的山核桃取物,并从分离釜1、2中回收夹带剂;停机从萃取釜中取出萃余物。The American hickory shells are preliminarily dried in the sun and then dried with hot air (70-90°C) until the moisture content is 5%, crushed into 5kg of 20-mesh hickory powder as raw material, and put it into a supercritical extraction kettle to heat up When the temperature reaches 60°C, start the plunger pump to pump CO 2 into the extraction kettle through the preheater. When the pressure reaches 30MPa, start the circulation; turn on the entrainer pump to make 10% acetone pass through the preheater and enter the extraction kettle at the same time; During the circulation process, CO2 and the extract are decompressed in the separator, and the extract is precipitated in the separator, and the CO2 is recycled. The separation pressure of the separation tank 1 is set at 8MPa and the temperature is 45 ° C. The separation tank 2 Set the separation pressure to 5MPa and the temperature to 30°C; after extraction for 2.5 hours, take out 35g of the extract from separation kettles 1 and 2, with a yield of 0.7%, and obtain 31g of pecan extract after drying at low temperature, and extract from Recover the entrainer in the separation kettle 1 and 2; stop the machine and take out the raffinate from the extraction kettle.

对提取物进行成分分析,结果同实施例1。UPLC法分析提取物的成分含量,其总甾醇含量为31.7%,β-谷甾醇含量为25.4%(即,总甾醇中β-谷甾醇的含量为80.12%),β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇比例为80.2:3.5:6.4:9.9。The extract is subjected to component analysis, and the result is the same as in Example 1. The content of the extract was analyzed by UPLC. The total sterol content was 31.7%, the β-sitosterol content was 25.4% (that is, the content of β-sitosterol in the total sterols was 80.12%), β-sitosterol, rock saponosterol , campesterol, stigmasterol ratio is 80.2:3.5:6.4:9.9.

实施例3、一种山核桃甾醇提取物的制备方法:Embodiment 3, a kind of preparation method of pecan sterol extract:

将云南山核桃仁粉碎后打成浆,经压榨除水初步晒干后,用微波干燥到水分含量为5%,粉碎成20目的山核桃仁粉末6kg,并将其放入超临界萃取釜中,升温到45℃,开动柱塞泵入CO2,通过预热器进入萃取釜中,当压力达到20MPa,开始循环;在循环过程中,CO2和萃取物在分离器中经减压,将萃取物在分离器中析出,CO2循环使用,分离釜1设定分离压力为6MPa、温度为35℃,分离釜2设定分离压力为5MPa、温度为30℃;萃取1h后,从分离釜1、2中取出萃取物60g,得率为1.0%,经低温干燥后,得到49g的山核桃甾醇提取物;停机并从萃取釜中取出萃余物。Grind the hickory kernels from Yunnan into pulp, press to remove water and preliminarily dry them in the sun, then dry them with microwaves until the water content is 5%, crush them into 6kg of 20-mesh hickory kernel powder, and put them into a supercritical extraction kettle , raise the temperature to 45°C, start the plunger to pump CO 2 into the extraction kettle through the preheater, and start the cycle when the pressure reaches 20MPa; during the cycle, CO 2 and the extract are decompressed in the separator, and the The extract is precipitated in the separator, and the CO2 is recycled. The separation pressure of the separation kettle 1 is set to 6MPa and the temperature is 35°C, and the separation pressure of the separation kettle 2 is set to 5MPa and the temperature is 30°C; 60g of the extract was taken out in 1 and 2, and the yield was 1.0%. After drying at low temperature, 49g of the pecan sterol extract was obtained; the machine was shut down and the raffinate was taken out from the extraction kettle.

对提取物进行成分分析,结果同实施例1。UPLC法分析提取物的成分含量,其总甾醇含量为37.1%,β-谷甾醇含量为32.8%(即,总甾醇中β-谷甾醇的含量为88.4%),β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间比例为88.5:2:7.5:2。The extract is subjected to component analysis, and the result is the same as in Example 1. The content of the extract was analyzed by UPLC. The total sterol content was 37.1%, and the β-sitosterol content was 32.8% (that is, the content of β-sitosterol in the total sterols was 88.4%). The ratio between campesterol and stigmasterol is 88.5:2:7.5:2.

实施例4、一种山核桃甾醇提取物的制备方法:Embodiment 4, a kind of preparation method of pecan sterol extract:

将湖南山核桃仁和壳磨碎后打成浆,经压榨除水后初步晒干后,用微波干燥到水分含量为5%,粉碎成20目的粉末6kg,并将其放入超临界萃取釜中,升温到50℃,开动柱塞泵泵入CO2,通过预热器进入萃取釜中,当压力达到到15MPa,开始循环;开启夹带剂泵,使10%的乙醇通过预热器后同时进入萃取釜;在循环过程中,CO2和萃取物在分离器中经减压,将萃取物在分离器中析出,CO2循环使用,分离釜1设定分离压力为7MPa、温度为40℃,分离釜2设定分离压力为5MPa、温度为30℃;萃取2.5h后,从分离釜1、2中取出萃取物90g,得率为1.8%,经低温干燥后,得到78g的山核桃甾醇提取物,从分离釜1、2中回收夹带剂,停机从萃取釜中取出萃余物。Grind Hunan hickory nuts and shells, beat them into pulp, press to remove water, dry them in the sun, dry them with microwave until the moisture content is 5%, grind them into 20 mesh powder 6kg, and put them into a supercritical extraction kettle , heat up to 50°C, start the plunger pump to pump CO 2 into the extraction kettle through the preheater, and start circulation when the pressure reaches 15MPa; turn on the entrainer pump, so that 10% ethanol enters the extraction tank at the same time after passing through the preheater Extraction tank; during the circulation process, CO2 and the extract are decompressed in the separator, and the extract is precipitated in the separator, and CO2 is recycled. The separation pressure of the separation tank 1 is set at 7MPa and the temperature is 40°C. The separation pressure of separation kettle 2 is set at 5MPa and the temperature is 30°C; after extraction for 2.5h, 90g of extract is taken out from separation kettle 1 and 2, and the yield is 1.8%. After low-temperature drying, 78g of pecan sterol extraction material, recover the entrainer from the separation tank 1, 2, shut down and take out the raffinate from the extraction tank.

对提取物进行成分分析,结果同实施例1。UPLC法分析提取物的成分含量,其总甾醇含量为27.3%,β-谷甾醇含量为22.4%(即,总甾醇中β-谷甾醇的含量为82.05%),β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间比例为81.9:6.5:3.8:7.8。The extract is subjected to component analysis, and the result is the same as in Example 1. The content of the extract was analyzed by UPLC method, the total sterol content was 27.3%, the β-sitosterol content was 22.4% (that is, the content of β-sitosterol in the total sterol was 82.05%), β-sitosterol, rock saponosterol , campesterol, stigmasterol ratio is 81.9:6.5:3.8:7.8.

实施例5、一种山核桃甾醇提取物的制备方法:Embodiment 5, a kind of preparation method of pecan sterol extract:

将贵州山核桃皮切碎后初步晒干后,用微波干燥到水分含量为5%,粉碎成20目的粉末5kg,并将其放入超临界萃取釜中,升温到50℃,开动柱塞泵泵入CO2,通过预热器进入萃取釜中,当压力达到到25MPa,开始循环;在循环过程中,CO2和萃取物在分离器中经减压,将萃取物在分离器中析出,CO2循环使用,分离釜1设定分离压力为8MPa、温度为45℃,分离釜2设定分离压力为5MPa、温度为30℃;萃取4h后,从分离釜1、2中取出萃取物45g,得率为0.9%,经低温干燥后,得到37g的山核桃甾醇提取物,停机并从萃取釜中取出萃余物。Chop the Guizhou hickory nut skin and preliminarily dry it in the sun, dry it with microwave until the moisture content is 5%, crush it into 5kg of 20-mesh powder, put it into a supercritical extraction kettle, raise the temperature to 50°C, and start the plunger pump Pump CO 2 into the extraction tank through the preheater. When the pressure reaches 25MPa, the circulation starts; during the circulation process, CO 2 and the extract are decompressed in the separator, and the extract is separated in the separator. CO2 is recycled, the separation pressure of separation kettle 1 is set to 8MPa, the temperature is 45°C, the separation pressure of separation kettle 2 is set to 5MPa, and the temperature is 30°C; after 4 hours of extraction, 45g of extract is taken out from separation kettle 1 and 2 , The yield was 0.9%. After drying at low temperature, 37g of the pecan sterol extract was obtained. Stop the machine and take out the raffinate from the extraction kettle.

对提取物进行成分分析,结果同实施例1。UPLC法分析提取物的成分含量,其总甾醇含量为22.9%,β-谷甾醇含量为19.8%(即,总甾醇中β-谷甾醇的含量为86.46%),β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间比例为86.6:2:8.7:3.6。The extract is subjected to component analysis, and the result is the same as in Example 1. The content of the extract was analyzed by UPLC. The total sterol content was 22.9%, and the β-sitosterol content was 19.8% (that is, the content of β-sitosterol in the total sterols was 86.46%). , campesterol, stigmasterol ratio is 86.6:2:8.7:3.6.

活性测试1、将实施例1所得的山核桃甾醇提取物进行如下性能检测Activity test 1, the Cargo sterol extract obtained in embodiment 1 is carried out to the following performance detection

山核桃甾醇提取物的抗炎作用:Anti-inflammatory effects of pecan sterol extract:

1)对巴豆油所致小鼠耳廓肿胀的影响1) Effect on ear swelling of mice induced by croton oil

小鼠按体重随机分成5组,每组10只,设置如下:①空白对照组:等体积生理盐水,0.8mL/20g;②阳性对照组:消炎痛10mg/kg;③高剂量组:200mg/kg的山核桃甾醇提取物;④中剂量组:100mg/kg的山核桃甾醇提取物;⑤低剂量组:50mg/kg的山核桃甾醇提取物。动物每天给药1次,连续7d(消炎痛仅给药1次,后面6天为生理盐水),末次给药后1h,小鼠右耳涂2%巴豆油0.02mL/只、致炎,4h后处死,沿耳廓剪下左右耳,以9mm环钻冲下左右耳片,称重,以左右耳片重量之差值作为肿胀率。The mice were randomly divided into 5 groups according to body weight, 10 in each group, and the settings were as follows: ①Blank control group: equal volume of normal saline, 0.8mL/20g; ②Positive control group: indomethacin 10mg/kg; ③High-dose group: 200mg/kg kg of pecan sterol extract; ④ medium dose group: 100 mg/kg of pecan sterol extract; ⑤ low dose group: 50 mg/kg of pecan sterol extract. Animals were administered once a day for 7 consecutive days (indomethacin was only administered once, and normal saline was used for the next 6 days). 1 hour after the last administration, the right ear of the mouse was coated with 0.02mL of 2% croton oil to induce inflammation for 4 hours Afterwards, they were put to death, and the left and right ears were cut along the auricles, and the left and right ear pieces were punched out with a 9mm trephine drill, and weighed. The difference in weight between the left and right ear pieces was used as the swelling rate.

备注说明:上述本发明山核桃甾醇提取物(以及“消炎痛”)无须用生理盐水溶解,直接给药。Remarks: The above-mentioned hickory nut sterol extract (and "indomethacin") of the present invention need not be dissolved in physiological saline, and can be administered directly.

实验结果表明,小鼠灌胃给予100mg/kg和200mg/kg剂量的山核桃甾醇提取物连续7d后,对巴豆油所致的耳廓肿胀具有显著(p<0.05)和极显著(p<0.01)的抑制作用,并呈明显的剂量依赖关系。The experimental results showed that after intragastric administration of 100mg/kg and 200mg/kg doses of pecan sterol extract to mice for 7 days, it had significant (p<0.05) and extremely significant (p<0.01) effects on the ear swelling caused by croton oil. ) in a dose-dependent manner.

表1山核桃甾醇提取物对小鼠巴豆油所致耳廓肿胀的影响

Figure BDA0000473328440000081
Table 1 Effect of hickory nut sterol extract on ear swelling caused by croton oil in mice
Figure BDA0000473328440000081

Figure BDA0000473328440000082
Figure BDA0000473328440000082

*p<0.05,**p<0.01,与对照组相比。 * p<0.05, ** p<0.01, compared to the control group.

2)对二甲苯所致小鼠耳廓肿胀的影响2) Effect of p-xylene-induced ear swelling in mice

小鼠按体重随机分成5组,每组10只,设置同上1。动物每天给药1次,连续7d(消炎痛仅给药1次),末次给药后30min,小鼠右耳涂二甲苯0.05mL/只、致炎,15min后处死,沿耳廓剪下左右耳,以9mm环钻冲下左右耳片,称重,以左右耳片重量之差值作为肿胀率。并与对照组比较,判断疗效。The mice were randomly divided into 5 groups according to body weight, 10 in each group, and the setting was the same as 1 above. The animals were administered once a day for 7 consecutive days (indomethacin was only administered once). 30 minutes after the last administration, the right ear of the mouse was coated with 0.05 mL of xylene to cause inflammation. After 15 minutes, it was killed, and the left and right ears were cut along the auricle. For ears, the left and right ear pieces were punched out with a 9mm trephine, weighed, and the difference in weight between the left and right ear pieces was used as the swelling rate. And compared with the control group to judge the curative effect.

表2显示,小鼠灌胃给予400mg/kg剂量的山核桃甾醇提取物连续7天后,对二甲苯所致耳廓肿胀具有显著(p<0.05)的抑制作用,中、低剂量时作用不明显。Table 2 shows that after intragastric administration of 400 mg/kg of hickory nut sterol extract to mice for 7 consecutive days, it has a significant (p<0.05) inhibitory effect on auricle swelling caused by xylene, and the effect is not obvious at medium and low doses .

表2山核桃甾醇提取物对小鼠二甲苯所致耳廓肿胀的影响 Table 2 Effect of hickory nut sterol extract on ear swelling caused by xylene in mice

Figure BDA0000473328440000092
Figure BDA0000473328440000092

*p<0.05,**p<0.01,与对照组相比。 * p<0.05, ** p<0.01, compared to the control group.

本发明采用超临界CO2流体萃取技术从山核桃及其加工废弃物中提取植物甾醇类提取物。不仅工艺操作简便,而且得到的山核桃甾醇提取物质量好,品质稳定。而且该提取物具有良好的消炎、降血脂和血胆固醇等功效,在化妆品、食品、保健品、药品中有广泛的应用前景。The invention adopts the supercritical CO2 fluid extraction technology to extract the phytosterol extract from the hickory nut and its processing waste. Not only the process is easy to operate, but also the quality of the obtained pecan sterol extract is good and stable. Moreover, the extract has good effects of anti-inflammation, lowering blood fat and blood cholesterol, etc., and has wide application prospects in cosmetics, food, health care products and medicines.

活性测试2、将上述实施例所得的山核桃甾醇提取物等同于上述活性测试1的方法进行检测,所得结果如下:Activity test 2, the method that the pecan sterol extract that above-mentioned embodiment gains is equal to above-mentioned activity test 1 detects, and obtained result is as follows:

表3、山核桃甾醇提取物对小鼠巴豆油所致耳廓肿胀的影响

Figure BDA0000473328440000093
Table 3, the effect of hickory nut sterol extract on the auricle swelling caused by mouse croton oil
Figure BDA0000473328440000093

*p<0.05,**p<0.01,与对照组相比。 * p<0.05, ** p<0.01, compared to the control group.

表4、山核桃甾醇提取物对小鼠二甲苯所致耳廓肿胀的影响

Figure BDA0000473328440000101
Table 4, the effect of hickory nut sterol extract on mouse auricle swelling caused by xylene
Figure BDA0000473328440000101

Figure BDA0000473328440000102
Figure BDA0000473328440000102

*p<0.05,**p<0.01,与对照组相比。 * p<0.05, ** p<0.01, compared to the control group.

最后,还需要注意的是,以上列举的仅是本发明的若干个具体实施例。显然,本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。Finally, it should be noted that the above examples are only some specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments, and many variations are possible. All deformations that can be directly derived or associated by those skilled in the art from the content disclosed in the present invention should be considered as the protection scope of the present invention.

Claims (10)

1.山核桃甾醇提取物在制备消炎物品中的应用。1. the application of hickory nut sterol extract in the preparation anti-inflammatory article. 2.根据权利要求1所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:所述山核桃甾醇提取物中总甾醇重量含量为10~50%,并且所述的总甾醇包括β-谷甾醇、岩皂甾醇、菜油甾醇和豆甾醇。2. the application of pecan sterol extract according to claim 1 in the preparation of anti-inflammatory articles is characterized in that: the total sterol weight content is 10~50% in the described pecan sterol extract, and described total sterol Including beta-sitosterol, rock soap sterol, campesterol and stigmasterol. 3.根据权利要求2所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:总甾醇中β-谷甾醇的重量含量为70-95%,并且β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比为70~95:1~10:2~12:1~15。3. the application of pecan sterol extract according to claim 2 in the preparation anti-inflammatory article is characterized in that: the weight content of β-sitosterol is 70-95% in the total sterols, and β-sitosterol, rock soap The weight ratio among sterol, campesterol and stigmasterol is 70-95:1-10:2-12:1-15. 4.根据权利要求3所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:该提取物中总甾醇重量含量为20-40%,并且总甾醇中β-谷甾醇的重量含量为75-90%。4. the application of pecan sterol extract according to claim 3 in the preparation anti-inflammatory article is characterized in that: total sterol weight content is 20-40% in this extract, and the weight of β-sitosterol in total sterol The content is 75-90%. 5.根据权利要求4所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比为75~90:2~10:2~10:2~11。5. the application of pecan sterol extract according to claim 4 in the preparation anti-inflammatory article is characterized in that: the weight ratio between β-sitosterol, rock saponosterol, campesterol, stigmasterol is 75~90: 2~10: 2~10: 2~11. 6.根据权利要求5所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:β-谷甾醇、岩皂甾醇、菜油甾醇、豆甾醇之间的重量比例为76.5:9.6:2.9:11。6. the application of pecan sterol extract according to claim 5 in the preparation anti-inflammatory article is characterized in that: the weight ratio between β-sitosterol, rock soap sterol, campesterol, stigmasterol is 76.5:9.6: 2.9:11. 7.根据权利要求1~6任一所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:山核桃甾醇提取物的制备方法包括以下步骤:7. according to the application of the hickory nut sterol extract described in any one of claims 1 to 6 in the preparation of anti-inflammatory articles, it is characterized in that: the preparation method of the hickory nut sterol extract comprises the following steps: 1)、将山核桃粉碎后作为原料,在分离釜中,于下述条件对原料进行超临界流体萃取:萃取剂为CO2,萃取压力为15~35MPa,萃取温度为40~70℃,分离温度为30~50℃,分离压力为4~8MPa,循环动态萃取1~5h;1) The hickory nuts are crushed as raw materials. In the separation kettle, the raw materials are subjected to supercritical fluid extraction under the following conditions: the extraction agent is CO 2 , the extraction pressure is 15-35 MPa, the extraction temperature is 40-70°C, and the separation The temperature is 30-50°C, the separation pressure is 4-8 MPa, and the dynamic extraction is 1-5 hours in circulation; 2)、从分离釜中取出萃取物,经干燥,从而获得山核桃甾醇提取物。2) Take out the extract from the separation kettle and dry it to obtain the pecan sterol extract. 8.根据权利要求7所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:8. the application of pecan sterol extract according to claim 7 in the preparation anti-inflammatory article is characterized in that: 步骤1)中的萃取压力为20~30MP,萃取温度为45~65℃,使用夹带剂,所述夹带剂的用量为山核桃重量的5~15%;所述夹带剂为C1~C4的醇类有机溶剂或C1~C4的酮类有机溶剂。The extraction pressure in step 1) is 20-30MP, the extraction temperature is 45-65°C, and an entrainer is used. The amount of the entrainer is 5-15% of the weight of the hickory; the entrainer is C1-C4 alcohol Organic solvents or C1-C4 ketone organic solvents. 9.根据权利要求1~6任一所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:将山核桃甾醇提取物制备成组合物,所述组合物由0.01-99.9wt%的山核桃甾醇提取物和作为余量的可接受载体组成。9. The application of the hickory nut sterol extract according to any one of claims 1 to 6 in the preparation of anti-inflammatory articles, characterized in that: the hickory nut sterol extract is prepared into a composition, and the composition consists of 0.01-99.9wt % of pecan sterol extract and acceptable carrier as the balance. 10.根据权利要求9所述的山核桃甾醇提取物在制备消炎物品中的应用,其特征在于:所述组合物为药物组合物、保健品组合物、食品组合物或化妆品组合物。10. The application of the pecan sterol extract according to claim 9 in the preparation of anti-inflammatory articles, characterized in that: the composition is a pharmaceutical composition, a health product composition, a food composition or a cosmetic composition.
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