WO2021136410A1 - 一种天然产物的脉冲压力冷萃方法 - Google Patents

一种天然产物的脉冲压力冷萃方法 Download PDF

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WO2021136410A1
WO2021136410A1 PCT/CN2020/141540 CN2020141540W WO2021136410A1 WO 2021136410 A1 WO2021136410 A1 WO 2021136410A1 CN 2020141540 W CN2020141540 W CN 2020141540W WO 2021136410 A1 WO2021136410 A1 WO 2021136410A1
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plant
pulse pressure
natural products
water
extraction
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PCT/CN2020/141540
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French (fr)
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赵靓
王永涛
廖小军
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中国农业大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids

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  • the invention relates to a cold extraction method of natural products, in particular to a pulse pressure cold extraction method of natural products.
  • solvent extraction that is, according to the solubility of the target in the solvent, select a solvent with high solubility for the target, insoluble or low solubility for the non-target, and selectively reduce the target
  • solvent extraction is divided into water method and organic solvent method. Since the target is generally divided into hydrophilic and lipophilic, the organic solvent method can be further divided into hydrophilic organic solvent method (such as ethanol, methanol, acetone method) and lipophilic Organic solvent method (such as petroleum ether, benzene, chloroform, ether, ethyl acetate, dichloroethane, propane, butane, etc.).
  • the water method is safer, it takes a long time to extract the target at low temperature and has low production efficiency.
  • problems such as poor selectivity for the target, serious degradation, and high energy consumption.
  • the organic solvent method has hidden food safety hazards due to organic solvent residues. Therefore, the development of efficient and safe natural product extraction methods is of great significance for effective use of biological resources, improving the safety of natural products, protecting the ecological environment, saving energy, and reducing labor costs.
  • microwave, ultrasonic, and high-voltage pulsed electric field technologies have significant degradation of the target during the extraction process; supercritical fluid technology is mainly limited to the extraction of weakly polar and non-polar substances in natural products; high-pressure carbon dioxide The technology is mainly limited to the extraction of polar and mid-polar substances; separate ultra-high pressure extraction usually uses higher processing pressure but lower efficiency.
  • the present invention provides a pulse pressure cold extraction method of natural products.
  • This method uses pulsed pressure to use water for cold extraction under low temperature conditions, which can avoid the degradation and oxidation of natural products in the traditional extraction process, effectively retain the functionality and activity of natural products, and improve extraction efficiency. It has a wide range of applications and is non-toxic and non-toxic. Harmful, green, energy-saving, environmentally friendly, and convenient for industrialized scale production.
  • the method is suitable for the cold extraction of various natural products of plant origin, including polar, neutral and non-polar natural products, and can realize the cold extraction of complex natural products. It is mostly used in the fields of agricultural products processing, food (including health food) processing, and extraction of active ingredients of Chinese medicinal materials.
  • the pulse pressure cold extraction method of natural products provided by the present invention includes:
  • the plant-derived substance rich in natural products is selected from at least one of plants and fruits containing natural active substances; specifically selected from those that can be used as food raw materials, herbal teas, and medicinal and edible raw materials. And at least one of plants containing natural active substances and fruits of Chinese medicinal materials; more specifically, at least one selected from blueberries, coffee, roses, tea, medlar, Dendrobium officinale and astragalus.
  • the natural product may be selected from at least one of various types of natural products of polar, neutral and non-polar; more specifically, it may be selected from caffeine, tea polyphenols, alkaloids, polysaccharides, saponins, flavonoids and At least one of trace elements.
  • the mesh number after crushing is 20-100 mesh; specifically, it can be 60 mesh;
  • the dosage ratio of the plant-derived substance rich in natural products to water is 1g:10-60mL; specifically, 1g:30mL, 1g:40mL or 1g:50mL;
  • the temperature of the water is 0-10°C; specifically, 0-4°C; more specifically, it can be 0-2°C;
  • the water is pure water.
  • the step 2) in the stirring and mixing step the temperature is 0-10°C;
  • the speed is 10-1000rpm; specifically 20rpm, 30rpm or 50rpm or 20-100rpm or 20-500rpm;
  • the time is 0-6h; specifically 0.5h or 0.2h or 0.5-5h or 0.5-2h or 0.5-1h;
  • the pulse pressure is divided into 2-5 stages of pulse pressure
  • the pressure of each stage is 50-300MPa; it can be 100MPa, 150MPa or 50-250MPa or 50-150MPa; the time is 0-20min; it can be 0.5min, 1min, 2min, 3min or 4min or 0.5-10min or 0.5 -15min; The temperature is 0-10°C;
  • the time interval of each stage of pressure treatment is 0-1h; specifically, it can be 1min, 2min or 0-30min or 0-10min or 0-5min;
  • the ambient temperature during the interval is 0-10°C. Specifically, it can be 4°C;
  • the pressure transmission medium of the pulse pressure cold extraction is water.
  • the present invention will be further described below in conjunction with specific embodiments, but the present invention is not limited to the following embodiments.
  • the methods are conventional methods unless otherwise specified.
  • the raw materials can be obtained from open commercial channels unless otherwise specified.
  • a method for cold water extraction of roses includes dissolving dried roses, stirring and mixing, and pulse pressure cold extraction.
  • the method for cold water extraction of roses includes the following steps:
  • the flexible packaging material After stirring and mixing, the flexible packaging material is used for filling and sealing, the first stage pressure condition is 100MPa, 4min; the second stage pressure condition is 50MPa, 1min; the third stage pressure condition is 150MPa, 2min; pressure treatment The temperature is less than 10°C; the pressure treatment interval of each stage is 2min; the pressure transmission medium is water.
  • the cold-extracted rose water prepared according to the method well retains the original aroma of the rose.
  • a method for cold extraction of caffeine includes crushing and dissolving coffee beans, stirring and mixing, and pulse pressure cold extraction.
  • the method for cold extraction of caffeine includes the following steps:
  • the first stage pressure condition is 50MPa, 3min; the second stage pressure condition is 150MPa, 1min; the third stage pressure condition is 100MPa, 2min; pressure treatment temperature 4°C; The pressure treatment interval of each stage is 1min; the pressure transmission medium is water.
  • the cold brew coffee product prepared by the method has a caffeine extraction rate of 70%.
  • a method for extracting natural products of Dendrobium officinale includes crushing and dissolving Dendrobium officinale, stirring and mixing, and pulse pressure cold extraction.
  • the method for extracting natural products of Dendrobium officinale includes the following steps:
  • the first stage pressure condition is 100MPa, 1min
  • the second stage pressure condition is 50MPa, 2min
  • the third stage pressure condition is 200MPa, 0.5min
  • the fourth stage The pressure condition is 50MPa, 1min
  • the pressure treatment temperature is 10°C; there is no interval between different stages of treatment
  • the pressure transmission medium is water.
  • the extraction rate of polysaccharides and alkaloids in the natural product extract of Dendrobium officinale obtained by the method is 80%.
  • the present invention uses a pulsed high pressure method to cold extract natural products, which can destroy plant cells during the cyclic pressure increase and pressure relief process, improve the dissolution efficiency of natural products, and save extraction time;
  • the pulsed high voltage method adopted in the present invention can also inactivate endogenous enzymes that have a degrading effect on natural products, and effectively retain the activity of natural products;
  • the present invention can avoid the problems of low extraction efficiency and high extraction pressure caused by the use of ultra-high pressure alone, and realizes greenness, energy saving and environmental protection.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

一种天然产物的脉冲压力冷萃方法，将富含天然产物的植物源物质破碎或保留原始形状溶于水中，得到植物源物质水溶液；再将植物源物质水溶液搅拌混匀，装入柔性包装材料，密封，随后进行脉冲压力冷萃。经过本发明方法处理后可实现各类植物源天然产物的冷萃，避免传统提取过程中天然产物的降解和氧化，有效保留天然产物功能性和活性，提高提取效率，适用范围广，便于工业化规模生产。

Description

一种天然产物的脉冲压力冷萃方法 技术领域
本发明涉及一种天然产物的冷萃方法，特别是涉及一种天然产物的脉冲压力冷萃方法。
背景技术
一般来说，天然产物的提取多采用溶剂浸提法，即根据目标物在溶剂中的溶解性，选用对目标物溶解度大、对非目标物不溶解或溶解度小的溶剂，选择性的将目标物从基质内溶出，继而溶入溶剂的方法。溶剂浸提发分为水法和有机溶剂法，由于目标物一般分为亲水性和亲脂性两种，有机溶剂法可进一步分为亲水有机溶剂法(如乙醇、甲醇、丙酮法)和亲脂有机溶剂法(如石油醚、苯、氯仿、乙醚、乙酸乙酯、二氯乙烷、丙烷、丁烷等)。其中水法虽然安全性较好，但存在低温时目标物提取耗时长，生产效率低的问题；而高温时又存在对目标物选择性差、降解严重、能耗高等问题。而有机溶剂法因有机溶剂残留而存在食品安全隐患。因此，开发高效、安全的天然产物提取方法对有效利用生物资源、提高天然产物安全性、保护生态环境、节约能源、降低劳动成本具有重要意义。
随着科研工作者对天然产物研究范围的扩大和深度的提高、消费者对天然产物生理功能的认识和对安全性的更高要求，以及生产者对日益扩大的天然产物消费市场的高度重视，创新的提取技术得以开发利用，如微波、超声波、高压脉冲电场、超临界流体、高压二氧化碳和超高压等。但是有研究发现，微波、超声波和高压脉冲电场技术在提取过程中存在对目标物显著降解的现象；超临界流体技术主要局限于对天然产物中弱极性和非极性物质的提取；高压二氧化碳技术主要局限于对极性和中极性物质的提取；单独的超高压提取通常采用的处理压力较高，但效率较低。
发明公开
为避免现有提取技术存在的诸多问题，本发明提供一种天然产物的脉冲压力冷萃方法。该方法是在低温条件下采用脉冲式压力利用水进行冷萃，能够避免传统提取过程中天然产物的降解和氧化，有效保留天然产物功能性和活性，提高提取效率，适用范围广，无毒无害，绿色、节能、环保，便于工 业化规模生产。
本方法适用于各类植物源天然产物的冷萃，包括极性、中性和非极性天然产物，并且可实现复合型天然产物的冷萃。多应用于农产品加工、食品(含保健食品)加工、中药材活性成分提取等领域。
本发明提供的天然产物的脉冲压力冷萃方法，包括：
1)将富含天然产物的植物源物质破碎或保留原始形状溶于水中，得到植物源物质水溶液；
2)将所述植物源物质水溶液搅拌混匀，装入柔性包装材料，密封，随后进行脉冲压力冷萃。
上述方法的步骤1)中，所述富含天然产物的植物源物质选自含有天然活性物质的植物和其果实中至少一种；具体选自能作为食品原料、花草茶、药食同源原料和中药材原料的含有天然活性物质的植物和其果实中至少一种；更具体选自蓝莓、咖啡、玫瑰花、茶叶、枸杞、铁皮石斛和黄芪中至少一种。
所述天然产物具体可选自极性、中性和非极性各类天然产物中至少一种；更具体可选自咖啡碱、茶多酚、生物碱、多糖类、皂苷类、黄酮类和微量元素中至少一种。
所述步骤1)中，破碎后的目数为20-100目；具体可为60目；
所述富含天然产物的植物源物质与水的用量比为1g:10-60mL；具体为1g:30mL、1g:40mL或1g:50mL；
所述水的温度为0-10℃；具体为0-4℃；更具体可为0-2℃；
所述水为纯净水。
所述步骤2)搅拌混匀步骤中，温度为0-10℃；
转速为10-1000rpm；具体为20rpm、30rpm或50rpm或20-100rpm或20-500rpm；
时间为0-6h；具体为0.5h或0.2h或0.5-5h或0.5-2h或0.5-1h；
所述步骤3)中，所述脉冲压力冷萃步骤中，所述脉冲压力共分为2-5个阶段的脉冲压力；
每一阶段的压强为50-300MPa；具体可为100MPa、150MPa或50-250MPa或50-150MPa；时间为0-20min；具体可为0.5min、1min、2min、3min或4min或0.5-10min或0.5-15min；温度为0-10℃；
每一阶段压力处理的时间间隔为0-1h；具体可为1min、2min或0-30min或0-10min或0-5min；
间隔期的环境温度为0-10℃。具体可为4℃；
所述脉冲压力冷萃的传压介质为水。
实施发明的最佳方式
下面结合具体实施例对本发明作进一步阐述，但本发明并不限于以下实施例。所述方法如无特别说明均为常规方法。所述原材料如无特别说明均能从公开商业途径获得。
实施例1
一种玫瑰花水冷萃方法，包括将干制玫瑰花溶解、搅拌混匀和脉冲压力冷萃。
其中，所述玫瑰花水冷萃的方法包括以下步骤:
(1)溶解：选用高品质干制玫瑰花，以1:40/g:mL的质量体积比加入4℃的纯净水；
(2)搅拌混匀：温度0-4℃，转速30rpm，时间0.5h；
(3)脉冲压力冷萃：搅拌混匀后采用柔性包材灌装、密封，第一阶段压力条件100MPa，4min；第二阶段压力条件50MPa，1min；第三阶段压力条件150MPa，2min；压力处理温度<10℃；各阶段压力处理间隔2min；传压介质为水。
按所述方法制得的冷萃玫瑰花水很好的保留了玫瑰花原始香气。
实施例2
一种冷萃取咖啡碱的方法，包括将咖啡豆破碎溶解、搅拌混匀和脉冲压力冷萃。
其中，所述冷萃取咖啡碱的方法包括以下步骤:
(1)破碎溶解：选用优质咖啡豆破碎至60目，以1:30/g:mL的质量体积比加入4℃的纯净水；
(2)搅拌混匀：温度0-4℃，转速20rpm，时间0.5h；
(3)脉冲压力提取：搅拌混匀后采用柔性包材灌装、密封，第一阶段压力 条件50MPa，3min；第二阶段压力条件150MPa，1min；第三阶段压力条件100MPa，2min；压力处理温度4℃；各阶段压力处理间隔1min；传压介质为水。
按所述方法制得的冷萃咖啡产品，咖啡碱提取率为70％。
实施例3
一种铁皮石斛天然产物提取方法，包括将铁皮石斛破碎溶解、搅拌混匀和脉冲压力冷萃。
其中，所述铁皮石斛天然产物提取方法包括以下步骤:
(1)破碎溶解：选用优质铁皮石斛破碎至40目，以1:50/g:mL的质量体积比加入0-2℃的纯净水；
(2)搅拌混匀：温度0-2℃，转速50rpm，时间0.2h；
(3)脉冲压力提取：搅拌混匀后柔性包材灌装、密封，第一阶段压力条件100MPa，1min；第二阶段压力条件50MPa，2min；第三阶段压力条件200MPa，0.5min；第四阶段压力条件50MPa，1min；压力处理温度均为10℃；不同阶段处理之间无间隔；传压介质为水。
按所述方法制得的铁皮石斛天然产物提取液中多糖类、生物碱类物质提取率为80％。
工业应用
本发明的有益效果在于：
1)本发明的整个环节在低温下进行，能够很好的保留天然产物活性和功能性；并且采用水作为冷萃介质，避免了有机溶剂提取的安全性问题；
2)本发明利用脉冲式高压方式对天然产物进行冷萃，在循环的升压和卸压过程中可实现对植物细胞的破坏，提高了天然产物溶出效率，节约了提取时间；
3)本发明采用的脉冲式高压方式还可以钝化对天然产物有降解作用的内源酶，有效保留天然产物的活性；
4)本发明能够避免单独使用超高压导致的提取效率低、提取压力过高等问题，实现了绿色、节能、环保。

Claims (6)

  1. 一种天然产物的脉冲压力冷萃方法，包括：
    1)将富含天然产物的植物源物质破碎或保留原始形状溶于水中，得到植物源物质水溶液；
    2)将所述植物源物质水溶液搅拌混匀，装入柔性包装材料，密封，随后进行脉冲压力冷萃。
  2. 根据权利要求1所述的方法，其特征在于：所述步骤1)中，所述富含天然产物的植物源物质选自含有天然活性物质的植物和其果实中至少一种；具体选自能作为食品原料、花草茶、药食同源原料和中药材原料的含有天然活性物质的植物和其果实中至少一种；更具体选自蓝莓、咖啡、玫瑰花、茶叶、枸杞、铁皮石斛和黄芪中至少一种。
  3. 根据权利要求1或2所述的方法，其特征在于：所述步骤1)中，破碎后的目数为20-100目；
    所述富含天然产物的植物源物质与水的用量比为1g:10-60mL；
    所述水的温度为0-10℃；
    所述水为纯净水。
  4. 根据权利要求1-3任一所述的方法，其特征在于：所述步骤2)搅拌混匀步骤中，温度为0-10℃；
    转速为10-1000rpm；
    时间为0-6h；
  5. 根据权利要求1-4任一所述的方法，其特征在于：所述步骤3)中，所述脉冲压力冷萃步骤中，所述脉冲压力共分为2-5个阶段的脉冲压力；
    每一阶段的压强为50-300MPa；时间为0-20min；温度为0-10℃；
    每一阶段压力处理的时间间隔为0-1h；
    间隔期的环境温度为0-10℃。
  6. 根据权利要求1-5任一所述的方法，其特征在于：所述脉冲压力冷萃的传压介质为水。
PCT/CN2020/141540 2019-12-31 2020-12-30 一种天然产物的脉冲压力冷萃方法 WO2021136410A1 (zh)

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CN111097188A (zh) * 2019-12-31 2020-05-05 中国农业大学 一种天然产物的脉冲压力冷萃方法
CN111528322A (zh) * 2020-05-18 2020-08-14 上海应用技术大学 一种抗疲劳功能性风味冷萃咖啡及其制备方法
CN113632867A (zh) * 2021-07-26 2021-11-12 中国农业大学 使用温和高压快速制备冷萃咖啡的方法

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