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CN101926452B - Wild jujube leaf total flavone extract and preparation method thereof - Google Patents

Wild jujube leaf total flavone extract and preparation method thereof Download PDF

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Publication number
CN101926452B
CN101926452B CN2009102602103A CN200910260210A CN101926452B CN 101926452 B CN101926452 B CN 101926452B CN 2009102602103 A CN2009102602103 A CN 2009102602103A CN 200910260210 A CN200910260210 A CN 200910260210A CN 101926452 B CN101926452 B CN 101926452B
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extract
ziziphi spinosae
extraction
jujube leaf
folium ziziphi
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CN101926452A (en
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王向红
桑亚新
周群标
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Heibei Agricultural University
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Heibei Agricultural University
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Abstract

A wild jujube leaf flavone extract is prepared through extracting concentrated general flavone extract from wild jujube leaf by alcohol extraction method, using alcohol solvent with a certain concentration, optimizing extraction time, extraction temp. and ratio of raw materials to liquid to obtain optimum extraction condition, preparing jujube leaf flavone extract liquid, filtering and concentrating. The crude extract has yield of more than 60%, and is rich in various nutritional components, such as total flavone content of more than 9%, protein content of more than 5%, total sugar content of more than 4%, and tannin content of 1%. The invention has simple preparation process, convenient operation and suitability for large-scale industrial production.

Description

酸枣叶总黄酮浸膏及其制备方法Sour jujube leaf total flavonoids extract and preparation method thereof

技术领域 technical field

本发明涉及一种利用野生酸枣叶制备黄酮浸膏的提取工艺,属食品科学与技术领域。  The invention relates to an extraction process for preparing flavonoid extract from wild jujube leaves, which belongs to the field of food science and technology. the

背景技术 Background technique

黄酮类化合物是广泛存在高等植物中的一类次生代谢类物质,具有很强的清除自由基能力,是药用植物的主要活性成分之一,相关药理和临床实验证实,黄酮类化合物具有广泛的药理功能,如不少治疗冠心病有效的中草药或活血化瘀类中药中均含有黄酮类化合物。由于该类化合物具有多种多样的生物活性和药理功能,且毒性较低,备受人们重视,成为功能性食品研究和开发利用的重点。黄酮类物质广泛的存在于植物的果实、花朵、叶片中,而且叶片在自然界中存在量大、来源广泛,因此从植物叶片中提取黄酮类物质近年来得到了广泛的发展,比如公开号为CN 101224224A,申请号200810010012.7“银杏叶中提取粗品黄酮和黄酮糖苷的方法”,是以银杏叶为原料提取黄酮类物质;公开号为CN 1597678A,申请号03133957.3“山楂叶总黄酮的提取方法”是以山楂叶为原料提取黄酮类物质,尚无酸枣叶黄酮提取研究的报道。  Flavonoids are a class of secondary metabolites that widely exist in higher plants. They have a strong ability to scavenge free radicals and are one of the main active ingredients of medicinal plants. Relevant pharmacological and clinical experiments have confirmed that flavonoids have a wide range of For example, many Chinese herbal medicines that are effective in treating coronary heart disease or traditional Chinese medicines that promote blood circulation and remove blood stasis contain flavonoids. Since this kind of compound has a variety of biological activities and pharmacological functions, and has low toxicity, it has attracted people's attention and has become the focus of research, development and utilization of functional foods. Flavonoids are widely found in fruits, flowers, and leaves of plants, and leaves have a large amount in nature and a wide range of sources. Therefore, the extraction of flavonoids from plant leaves has been widely developed in recent years. For example, the publication number is CN 101224224A , Application No. 200810010012.7 "Method for Extracting Crude Flavonoids and Flavone Glycosides from Ginkgo Leaf", which uses Ginkgo biloba as raw material to extract flavonoids; The leaves are used as raw materials to extract flavonoids, but there is no report on the extraction of flavonoids from jujube leaves. the

酸枣又名山枣,生长在我国北方地区多年生灌木。在我国北方有较大面积的野生酸枣林,资源非常丰富。酸枣的花果、枝叶及种仁都极具药理营养价值,目前对于酸枣仁黄酮的研究比较充分,而对于枣叶的开发利用尚属空白阶段。  Sour jujube, also known as wild jujube, is a perennial shrub that grows in northern my country. There is a large area of wild jujube forest in northern my country, and the resources are very rich. The flowers, fruits, branches, leaves and kernels of Zizyphus jujuba have great pharmacological nutritional value. At present, the research on the flavonoids of Zizyphus jujuba is relatively sufficient, but the development and utilization of jujube leaves is still in a blank stage. the

本发明采用溶剂对酸枣叶总黄酮进行提取测定,旨在找到一个提取酸枣叶中总黄酮的适宜方法,为酸枣产品的深度开发利用提供一个科学有效、便于规模化生产的制备工艺,同时也为山野资源的综合开发利用提供了新的途径。  The present invention uses a solvent to extract and measure the total flavonoids in spiny jujube leaves, aiming to find a suitable method for extracting the total flavonoids in spiny jujube leaves, and to provide a scientific and effective preparation process for the deep development and utilization of spiny jujube products, which is also convenient for large-scale production. The comprehensive development and utilization of mountain resources provides a new way. the

发明内容 Contents of the invention

本发明的目的在于利用野生酸枣叶,优化提取条件,从而获取较高含量的酸枣叶总黄酮浸膏,为酸枣相关产品的产业化开发开辟更广阔的市场前景。  The purpose of the present invention is to utilize wild spiny jujube leaves and optimize extraction conditions to obtain a higher content of total flavonoid extract from spiny jujube leaves, and to open up a broader market prospect for the industrial development of spiny jujube related products. the

工艺流程图见说明书附图,具体过程如下:  See the accompanying drawings for the process flow chart, and the specific process is as follows:

(1)酸枣叶干燥粉碎  (1) Dried jujube leaves and crushed

取野生酸枣叶105℃杀青15min,65℃通风干燥至恒重后粉碎。  Take the wild jujube leaves, fix them at 105°C for 15 minutes, ventilate and dry them at 65°C until they reach a constant weight, and then pulverize them. the

(2)脱脂酸枣叶粉制备  (2) Preparation of defatted jujube leaf powder

将干燥粉碎的酸枣叶粉末,用其质量5倍体积的石油醚回流浸提1.5h脱脂,将脱脂后的酸枣叶粉进行脱溶剂,获得脱脂酸枣叶粉。  The dried and pulverized spiny jujube leaf powder is degreased by reflux leaching with 5 times the volume of petroleum ether for 1.5 h, and the defatted spiny jujube leaf powder is desolventized to obtain defatted spiny jujube leaf powder. the

(2)酸枣叶粗提取物制备  (2) Preparation of Crude Extract of Jujube Leaves

称取一定量脱脂酸枣叶粉,采用体积比为50-80%乙醇溶剂浸提1-3h,浸提温度50-80℃,料液比1∶30-1∶60。提取完成后,过滤弃去沉淀,合并提取液,并于低于60℃的条件下真空减压浓缩,待提取物中可溶性固形物达到40%时,获得膏状浓缩物(也可将其进行真空干燥后获得粉状粗产品)。此外,也可以用大孔吸附树脂进行精制,获得纯度更高的酸枣叶黄酮制品。  A certain amount of defatted jujube leaf powder is weighed, extracted with an ethanol solvent having a volume ratio of 50-80% for 1-3 hours, the extraction temperature is 50-80° C., and the ratio of solid to liquid is 1:30-1:60. After the extraction is completed, filter and discard the precipitate, combine the extracts, and concentrate under reduced pressure under vacuum at a temperature lower than 60°C. When the soluble solids in the extract reach 40%, a paste-like concentrate is obtained (it can also be processed The powdery crude product was obtained after vacuum drying). In addition, macroporous adsorption resin can also be used for refining to obtain jujube leaf flavonoid products with higher purity. the

(3)产品主要技术指标  (3) Main technical indicators of the product

产品为棕黄色膏状物,略苦。酸枣叶总黄酮浸膏得率≥60%,总黄酮含量≥9%,总黄酮提取率≥78%,蛋白质含量≥5%、总糖含量≥4%、丹宁含量1%。  The product is a brownish-yellow paste, slightly bitter. Extraction rate of total flavonoids from jujube leaves is ≥60%, total flavonoid content is ≥9%, total flavonoid extraction rate is ≥78%, protein content is ≥5%, total sugar content is ≥4%, and tannin content is 1%. the

(4)检测方法  (4) Detection method

采用碱性NaNO2-Al(NO3)3显色法,以芦丁为标准品于波长510nm处测量样品吸光值,根据标准曲线计算出酸枣叶总黄酮含量。  Alkaline NaNO 2 -Al(NO 3 ) 3 chromogenic method was used to measure the absorbance of the samples at a wavelength of 510nm with rutin as a standard, and the total flavonoid content of jujube leaves was calculated according to the standard curve.

具体实施方式 Detailed ways

本发明通过以下实施例进一步详述,下述实施例是说明性的,不是限定性的,不能以下述实施例来限定本发明的保护范围。  The present invention is further described in detail by the following examples, which are illustrative, not restrictive, and the protection scope of the present invention cannot be limited by the following examples. the

将干燥的酸枣叶粉碎成粉末,用其质量5倍体积的石油醚回流浸提1.5h脱脂,将脱脂后的酸枣叶粉进行脱溶剂,获得脱脂酸枣叶粉。称取定量干燥的脱脂酸枣叶粉术,加入60%(体积比)的乙醇溶液,于67℃水浴提取1.5h,乙醇用量为料液比1∶50。提取完成后进行过滤,收集合并滤液。将上述酸枣叶提取液离心除杂,收集上清液待用。将上清液进行真空减压浓缩,回收乙醇。浓缩温度为60℃,真空度-0.1~-0.06MPa,直至浓缩液可溶性固形物达到40%止。(亦可将膏状浓缩液冷冻干燥,粉碎,制成粉末状酸枣叶总黄酮粗提物)。其得率为61.5%,膏状物中酸枣叶总黄酮含量为9.1%,蛋白质5.5%、总糖4.3%、丹宁1%。  Grinding the dried jujube leaves into powder, reflux extracting with 5 times the volume of petroleum ether for degreasing for 1.5 h, and desolventizing the degreased jujube leaf powder to obtain defatted jujube leaf powder. Weigh the quantitatively dried defatted jujube leaf powder, add 60% (volume ratio) ethanol solution, and extract in a water bath at 67° C. for 1.5 h, and the amount of ethanol is a solid-liquid ratio of 1:50. After the extraction is completed, filter and collect the combined filtrate. Centrifuge the extract of jujube leaves above to remove impurities, and collect the supernatant for later use. The supernatant was concentrated under reduced pressure in vacuo to recover ethanol. The concentration temperature is 60°C, the vacuum degree is -0.1~-0.06MPa, until the soluble solid content of the concentrated solution reaches 40%. (The paste concentrate can also be freeze-dried and pulverized to make the crude extract of total flavonoids from Suanzao leaves). The yield rate is 61.5%. The content of total flavonoids in jujube leaves in the paste is 9.1%, protein is 5.5%, total sugar is 4.3%, and tannin is 1%. the

Claims (1)

1. Folium Ziziphi Spinosae flavones extract making method is characterized in that comprising following preparation process:
(1) gets the Wild jujube leaf and complete, 80-120 ℃ of the temperature that completes, fixation time 10-30min; After 65 ℃ of following air seasoning to constant weights, pulverize, degreasing, degreasing solvent is sherwood oil or solvent oil; Folium Ziziphi Spinosae powder after the degreasing is carried out desolventizing, obtain degreasing Folium Ziziphi Spinosae powder;
(2) with 50-80% ethanol (volume ratio) lixiviate step (1) Folium Ziziphi Spinosae powder; Extract the pure soluble components in the Folium Ziziphi Spinosae; Obtain extracting solution, extraction time is 1-3h, extraction temperature 50-80 ℃; Solid-liquid ratio is 1: 30-1: 60, and any method in percolation, single-stage pickling process, multistage pickling process, continuous countercurrent extraction and the circumfluence method is taked in lixiviate;
(3) extracting solution that obtains of step (2) concentrates and reclaims ethanol and process Folium Ziziphi Spinosae flavones medicinal extract, wherein general flavone content >=9%.
CN2009102602103A 2009-12-25 2009-12-25 Wild jujube leaf total flavone extract and preparation method thereof Expired - Fee Related CN101926452B (en)

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CN104547104B (en) * 2013-10-24 2017-09-08 沈阳药科大学 Ramulus Ziziphi Spinosae leaf extract and its preparation method and application
CN105232669B (en) * 2015-11-05 2019-05-17 山西大学 A kind of wild jujube leaf flavone extract and its preparation method and application
CN105884842B (en) * 2016-01-28 2021-03-12 塔里木大学 Preparation of quercetin-3-O-alpha-L-arabinose- (1 → 2) -alpha-L-rhamnoside from red date leaves and application thereof
CN107951936A (en) * 2017-11-16 2018-04-24 金华市飞凌生物科技有限公司 There is the wild jujube extract for improving sleep
CN108419870A (en) * 2018-03-15 2018-08-21 洋县鹮居花茶产业发展有限公司 A kind of preparation method of chrysanthemum tea
CN110801014A (en) * 2019-11-29 2020-02-18 恩施硒禾生物科技有限公司 Method for preparing selenium-rich health food by using kudzu leaf extract
CN117205254B (en) * 2023-10-23 2024-09-06 河北瑞龙生物科技有限公司 Extraction method of wild jujube branch and leaf extract

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Non-Patent Citations (2)

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