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CN106749151B - Method for rapidly extracting blueberry pomace anthocyanin - Google Patents

Method for rapidly extracting blueberry pomace anthocyanin Download PDF

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CN106749151B
CN106749151B CN201611059315.9A CN201611059315A CN106749151B CN 106749151 B CN106749151 B CN 106749151B CN 201611059315 A CN201611059315 A CN 201611059315A CN 106749151 B CN106749151 B CN 106749151B
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anthocyanin
pomace
blueberry
acetic acid
blueberry pomace
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CN106749151A (en
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李斌
高凝轩
矫馨瑶
孟宪军
张琦
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Shenyang Agricultural University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0096Purification; Precipitation; Filtration

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract

本发明涉及一种蓝莓果渣花青素的快速提取方法,本发明以冷冻蓝莓果渣为原料,通过打浆机打成浆状,在一定温度下使用超高压装置处理后,向果渣中添加果胶酶、半纤维素酶、纤维素酶酶解,酶解后与乙醇‑乙酸‑水溶剂混合,并使用高压均质机处理提取花青素,通过离心机将果渣与花青素提取液分离,并使用减压浓缩的方式出去提取液中乙醇和乙酸后,放入真空冷冻干燥机中冻干制得蓝莓果渣花青素。本发明提供的技术方案工艺操作简单、周期短较,成本较低、污染较小,适合大批量连续化生产,实现了蓝莓的综合利用,具有良好的应用前景。The invention relates to a method for rapidly extracting anthocyanin from blueberry pomace. The invention uses frozen blueberry pomace as a raw material, is beaten into pulp by a beater, and is treated with an ultra-high pressure device at a certain temperature, and then added to the pomace. Pectinase, hemicellulase, and cellulase enzymatic hydrolysis, mixed with ethanol-acetic acid-water solvent after enzymatic hydrolysis, and processed with a high-pressure homogenizer to extract anthocyanin, and the pomace and anthocyanin were extracted by a centrifuge The liquid is separated and concentrated under reduced pressure to remove ethanol and acetic acid in the extract, and then put into a vacuum freeze dryer for freeze-drying to obtain blueberry pomace anthocyanins. The technical solution provided by the invention has simple process operation, short cycle, low cost and less pollution, is suitable for large-scale continuous production, realizes comprehensive utilization of blueberries, and has good application prospects.

Description

一种蓝莓果渣花青素的快速提取方法A kind of rapid extraction method of blueberry pomace anthocyanin

技术领域technical field

本发明涉及一种蓝莓果渣花青素的快速提取方法。The invention relates to a rapid extraction method of anthocyanin from blueberry pomace.

背景技术Background technique

蓝莓作为一种风味品质优良、营养价值高的小浆果,具较高营养保健价值和经济价值,在欧美等国家受到普遍欢迎,已经渐发展成为第三代新兴水果,具有很高的经济效益。花青素是纯天然的有效的抗氧化剂,并且具有保护视力、对糖尿病和心血管疾病有治疗的作用。蓝莓中花青素的含量较高,而且大部分存在于果渣中,且其具有良好的生理功能,因此是花青素的良好来源。传统提取方法使用水、醇等溶剂,通过加热、超声波辅助等工艺提取花青素。由于热处理对花青素稳定性具有极大影响,因此传统提取方法在提取过程中会对花青素造成极大的损失。此外,传统工艺需要提取时间相对较长,能耗较大,不利于连续生产。As a small berry with good flavor and quality and high nutritional value, blueberry has high nutritional value and economic value. Anthocyanins are all-natural and potent antioxidants that protect vision, treat diabetes and cardiovascular disease. The content of anthocyanins in blueberries is high, and most of them exist in the pomace, and they have good physiological functions, so they are a good source of anthocyanins. The traditional extraction method uses solvents such as water and alcohol, and extracts anthocyanins through processes such as heating and ultrasonic assistance. Since heat treatment has a great influence on the stability of anthocyanins, traditional extraction methods will cause great loss of anthocyanins during the extraction process. In addition, the traditional process requires relatively long extraction time and large energy consumption, which is not conducive to continuous production.

发明内容SUMMARY OF THE INVENTION

为了克服蓝莓果渣花青素提取过程中,周期长、花青素损失大的技术问题,本发明的目的是提供一种蓝莓果渣花青素的快速提取方法,采用超高压处理与高压均质方式的提取花青素,采用非热加工的方式提取蓝莓花青素,缩短提取时间,实现蓝莓花青素的连续化生产,且成本低廉,无污染,所生产的蓝莓花青素杂质少,纯净度高。In order to overcome the technical problems of long period and large anthocyanin loss in the extraction process of blueberry pomace anthocyanin, the purpose of the present invention is to provide a rapid extraction method of blueberry pomace anthocyanin, which adopts ultra-high pressure treatment and high pressure homogenization. The method of extracting anthocyanins in a quality way, extracting blueberry anthocyanins by non-thermal processing, shortens the extraction time, realizes continuous production of blueberry anthocyanins, and has low cost, no pollution, and the produced blueberry anthocyanins have less impurities. , high purity.

本发明提供的蓝莓果渣花青素的快速提取方法如下:The rapid extraction method of blueberry pomace anthocyanins provided by the invention is as follows:

操作工序:Operation procedure:

冷冻蓝莓果渣→解冻→打浆→超高压处理→乙醇-乙酸-水溶液浸提→高压均质处理→离心分离过滤→花青素提取液→减压浓缩→真空冷冻干燥→产品。Frozen blueberry pomace → thawing → beating → ultra-high pressure treatment → ethanol-acetic acid-water solution extraction → high pressure homogenization treatment → centrifugal separation filtration → anthocyanin extract → reduced pressure concentration → vacuum freeze drying → product.

具体操作过程为:The specific operation process is as follows:

(1)冷冻蓝莓果渣,解冻后用匀浆机打成匀浆,并使用超高压装置进行超高压处理;(1) Frozen blueberry pomace, after thawing, use a homogenizer to homogenize, and use an ultra-high pressure device for ultra-high pressure treatment;

(2)向步骤(1)处理后所得果渣中加入重量比例如下的成分:5‰果胶酶、3‰半纤维素酶、3‰纤维素酶,于50℃下酶解2h;(2) adding the following ingredients by weight to the pomace obtained after the treatment in step (1): 5‰ pectinase, 3‰ hemicellulase, 3‰ cellulase, and enzymatically hydrolyzed at 50° C. for 2 hours;

(3)酶解后加入乙醇-乙酸-水的混合溶液,乙醇-乙酸-水的体积比为40:10:50,其物料比为1 g:5 mL,混合均匀后使用高压均质机处理;(3) After enzymatic hydrolysis, add a mixed solution of ethanol-acetic acid-water, the volume ratio of ethanol-acetic acid-water is 40:10:50, and the material ratio is 1 g:5 mL. After mixing evenly, use a high-pressure homogenizer to process ;

(4)将步骤(3)所得到的浑浊液通过离心机分离过滤果渣和花青素提取液,并将花青素提取通过减压旋转蒸发装置除去乙醇及乙酸;(4) the turbid liquid obtained in step (3) is separated and filtered by a centrifuge and the anthocyanin extract, and the anthocyanin is extracted by a vacuum rotary evaporator to remove ethanol and acetic acid;

(5)将步骤(4)所得花青素水溶液使用真空冷冻干燥机中冻干,制得蓝莓花青素粉末。(5) The anthocyanin aqueous solution obtained in step (4) is freeze-dried in a vacuum freeze dryer to obtain blueberry anthocyanin powder.

本发明取得的有益效果主要包括:The beneficial effects obtained by the present invention mainly include:

1.采用超高压处理的方式,在非热加工的条件下,极大的破坏了蓝莓果渣的组织结构,同时使用酸性的乙醇溶液与蓝莓果渣进行混合,为后续的花青素的快速提取,创造了极为有利的条件。1. Using ultra-high pressure treatment, under the condition of non-thermal processing, the tissue structure of blueberry pomace is greatly destroyed, and at the same time, an acidic ethanol solution is used to mix with blueberry pomace, which is the rapidity of subsequent anthocyanins. Extraction creates extremely favorable conditions.

2.使用高压均质的的提取方式,配合有机溶剂提取液,可在没有加热的条件下,短时内将蓝莓果渣中花青素充分溶于有机溶剂,提取时间短,极大的缩短了生产周期,降低了能耗,提取温度低,所得到的蓝莓花青素粉末提取量高、纯净度高、杂质少。2. Using the high-pressure homogeneous extraction method, combined with the organic solvent extraction solution, the anthocyanin in the blueberry pomace can be fully dissolved in the organic solvent in a short time without heating, and the extraction time is short and greatly shortened. The production cycle is shortened, the energy consumption is reduced, the extraction temperature is low, and the obtained blueberry anthocyanin powder has high extraction quantity, high purity and less impurities.

具体实施方式Detailed ways

实施例1Example 1

取冻藏蓝莓果渣1kg,于常温下解冻后使用匀浆机打成匀浆,置于超高压装置中于350MPa,40℃下处理5min。向超高压处理后的果渣中加入5g果胶酶、3g半纤维素酶、3g纤维素酶,并于50℃下酶解2h。将酶解后的果渣加入5L乙醇-乙酸-水(40:10:50,v/v/v)溶液,使用高压均质机于2000转/min下处理7min。将高压均质后所得到的浑浊液通过离心机分离果渣和花青素提取液,并将花青素提取液通过减压旋转蒸发装置,于45℃下除去乙醇及乙酸,得蓝莓果渣花青素水溶液。将花青素水溶液置于真空冷冻干燥机中冻干,制得到蓝莓果渣花青素粉末4.8g。Take 1kg of frozen blueberry pomace, thaw it at room temperature, use a homogenizer to make it into a homogenate, and place it in an ultra-high pressure device at 350MPa and 40°C for 5min. 5 g of pectinase, 3 g of hemicellulase, and 3 g of cellulase were added to the pomace treated with ultra-high pressure, and enzymatically hydrolyzed at 50 °C for 2 h. Add 5 L of ethanol-acetic acid-water (40:10:50, v/v/v) solution to the enzymatically hydrolyzed pomace, and use a high-pressure homogenizer to process at 2000 rpm for 7 min. The turbid liquid obtained after high pressure homogenization is separated from the pomace and anthocyanin extract by a centrifuge, and the anthocyanin extract is passed through a vacuum rotary evaporation device to remove ethanol and acetic acid at 45 ° C to obtain blueberry pomace. Aqueous solution of anthocyanin. The anthocyanin aqueous solution was lyophilized in a vacuum freeze dryer to obtain 4.8 g of blueberry pomace anthocyanin powder.

实施例2Example 2

取冻藏蓝莓果渣10kg,于常温下解冻后使用匀浆机打成匀浆,置于超高压装置中于350MPa,40℃下处理7min。向超高压处理后的果渣中加入50g果胶酶、30g半纤维素酶、30g纤维素酶,并于50℃下酶解2h。将酶解后的果渣加入50L乙醇-乙酸-水(40:10:50,v/v/v)溶液,使用高压均质机于2000转/min下处理7min。将高压均质后所得到的浑浊液通过离心机分离果渣和花青素提取液,并将花青素提取液通过减压旋转蒸发装置,于45℃下除去乙醇及乙酸,得蓝莓果渣花青素水溶液。将花青素水溶液置于真空冷冻干燥机中冻干,制得到蓝莓果渣花青素粉末49.5g。Take 10kg of frozen blueberry pomace, thaw it at room temperature, use a homogenizer to make it into a homogenate, and place it in an ultra-high pressure device at 350MPa and 40°C for 7min. 50 g of pectinase, 30 g of hemicellulase, and 30 g of cellulase were added to the pomace treated with ultra-high pressure, and enzymatically hydrolyzed at 50° C. for 2 h. Add 50 L of ethanol-acetic acid-water (40:10:50, v/v/v) solution to the enzymatically hydrolyzed pomace, and use a high-pressure homogenizer to process at 2000 rpm for 7 min. The turbid liquid obtained after high pressure homogenization is separated from the pomace and anthocyanin extract by a centrifuge, and the anthocyanin extract is passed through a vacuum rotary evaporation device to remove ethanol and acetic acid at 45 ° C to obtain blueberry pomace. Aqueous solution of anthocyanin. The anthocyanin aqueous solution was lyophilized in a vacuum freeze dryer to obtain 49.5 g of blueberry pomace anthocyanin powder.

实施例3Example 3

取冻藏蓝莓果渣20kg,于常温下解冻后使用匀浆机打成匀浆,置于超高压装置中于350MPa,40℃下处理7min。向超高压处理后的果渣中加入100g果胶酶、60g半纤维素酶、60g纤维素酶,并于50℃下酶解2h。将酶解后的果渣加入100L乙醇-乙酸-水(40:10:50,v/v/v)溶液,使用高压均质机于2000转/min下处理7min。将高压均质后所得到的浑浊液通过离心机分离果渣和花青素提取液,并将花青素提取液通过减压旋转蒸发装置,于45℃下除去乙醇及乙酸,得蓝莓果渣花青素水溶液。将花青素水溶液置于真空冷冻干燥机中冻干,制得到蓝莓果渣花青素粉末99.3g。Take 20kg of frozen blueberry pomace, thaw it at room temperature, use a homogenizer to make it into a homogenate, and place it in an ultra-high pressure device at 350MPa and 40°C for 7min. 100 g of pectinase, 60 g of hemicellulase, and 60 g of cellulase were added to the pomace treated with ultra-high pressure, and enzymatically hydrolyzed at 50° C. for 2 h. Add 100 L of ethanol-acetic acid-water (40:10:50, v/v/v) solution to the enzymatically hydrolyzed pomace, and use a high-pressure homogenizer to process at 2000 rpm for 7 min. The turbid liquid obtained after high pressure homogenization is separated from the pomace and anthocyanin extract by a centrifuge, and the anthocyanin extract is passed through a vacuum rotary evaporation device to remove ethanol and acetic acid at 45 ° C to obtain blueberry pomace. Aqueous solution of anthocyanin. The anthocyanin aqueous solution was lyophilized in a vacuum freeze dryer to obtain 99.3 g of blueberry pomace anthocyanin powder.

Claims (3)

1.一种蓝莓果渣花青素的快速提取方法,其特征在于,具体包括以下步骤:1. a rapid extraction method of blueberry pomace anthocyanin, is characterized in that, specifically comprises the following steps: (1)冷冻蓝莓果渣,解冻后用匀浆机打成匀浆,并使用超高压装置进行超高压处理,所述超高压处理为:压力350MPa,温度为40℃,处理时间为5min;(1) Frozen blueberry pomace, after thawing, use a homogenizer to make a homogenate, and use an ultra-high pressure device to carry out ultra-high pressure treatment, the ultra-high pressure treatment is: pressure 350MPa, temperature is 40 ℃, and the treatment time is 5min; (2)向步骤(1)处理后所得果渣中加入重量比例如下的成分:5‰果胶酶、3‰半纤维素酶、3‰纤维素酶,于50℃下酶解2h;(2) adding the following ingredients by weight to the pomace obtained after the treatment in step (1): 5‰ pectinase, 3‰ hemicellulase, 3‰ cellulase, and enzymatically hydrolyzed at 50° C. for 2 hours; (3)酶解后加入乙醇-乙酸-水的混合溶液,乙醇-乙酸-水的体积比为40:10:50,其物料比为1 g:5 mL,混合均匀后使用高压均质机进行提取,转数为2000转/min,提取时间为7-10min;(3) After enzymatic hydrolysis, add a mixed solution of ethanol-acetic acid-water, the volume ratio of ethanol-acetic acid-water is 40:10:50, and the material ratio is 1 g:5 mL. Extraction, the number of revolutions is 2000 revolutions/min, and the extraction time is 7-10min; (4)将步骤(3)所得到的浑浊液通过离心机分离过滤果渣和花青素提取液,并将花青素提取通过减压旋转蒸发装置除去乙醇及乙酸;(4) the turbid liquid obtained in step (3) is separated and filtered by a centrifuge and the anthocyanin extract, and the anthocyanin is extracted by a vacuum rotary evaporator to remove ethanol and acetic acid; (5)将步骤(4)所得花青素水溶液使用真空冷冻干燥机中冻干,制得蓝莓花青素粉末。(5) The anthocyanin aqueous solution obtained in step (4) is freeze-dried in a vacuum freeze dryer to obtain blueberry anthocyanin powder. 2.根据权利要求1所述的一种蓝莓果渣花青素的快速提取方法,其特征在于,所述步骤(4)中离心机的过滤滤网目数为200目,减压旋转蒸发装置的减压浓缩温度为45℃。2. The method for rapidly extracting anthocyanins from blueberry pomace according to claim 1, wherein in the step (4), the filter mesh of the centrifuge is 200 meshes, and the decompression rotary evaporation device The temperature for concentration under reduced pressure was 45 °C. 3.根据权利要求1所述的一种蓝莓果渣花青素的快速提取方法,其特征在于,所述步骤(1)-(5)中料液温度控制在50℃以下。3 . The method for rapidly extracting anthocyanins from blueberry pomace according to claim 1 , wherein in the steps (1)-(5), the temperature of the feed liquid is controlled below 50° C. 4 .
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