• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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  • 引用文献
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    • 专利摘要:
    Procedure for obtaining oleuropein. The present invention relates to a process for obtaining oleuropein from olive leaves comprising the following steps: a) drying of the olive leaves; b) pelletizing the dried leaves obtained in step (a); and c) solid/liquid extraction of the pellets obtained in step (b) with a solvent selected from water, methanol, ethanol and any of their mixtures. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2631004A2
    申请号:ES201630209
    申请日:2016-02-24
    公开日:2017-08-25
    发明作者:Angeles GUINDA GARÍN；Mirela RADA；José María CASTELLANO OROZCO
    申请人:Consejo Superior de Investigaciones Cientificas CSIC；
    IPC主号:
    专利说明:

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    Procedure for obtaining oleuropein DESCRIPTION
    The present invention relates to a process for obtaining oleuropein, therefore, it can be framed in the technical field of the extraction of natural products from the olive tree.
    STATE OF THE TECHNIQUE
    Oleuropein is a phenolic component present in the pulp of olives and also in olive leaves (European Olea).
    The pharmacological properties of olive oil, olives and olive leaves have been recognized in medicine and in a healthy diet due to their phenol content.
    Numerous studies have shown that oleuropein has a wide range of pharmacological and health promoting properties, including its effects as antioxidant, anti-inflammatory, anti-atherogenic, anti-cancer, antimicrobial and antiviral. Specific reviews have been published on the pharmacological effects of olive biophenols and the protective action of the oleuropein secoiridoid in preclinical studies on cardiovascular and metabolic diseases (Bulotta et al. J. Transl. Med. 2014, 12, 219; Obied et al Pharmacology of olive biophenols.In: JC Fishbein, & JM Heilman (Eds.), Advances in molecular toxicology 2012, 195-223, Amsterdam: Elsevier).
    For the reasons stated above, oleuropein is a highly valued food supplement.
    There are various procedures for obtaining oleuropein in the state of the art, which are mainly extraction procedures by maceration of parts of the olive tree that comprise oleuropein, mainly from green olives. However, procedures for extracting oleuropein from olive leaves have also been described. For example, Job Nexar-QH (An Fac med. 2013, 74 (4), 285290) describes the preparation of a hydroalcoholic extract of European Olea leaves.
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    For this, the leaves are dried at room temperature and pulverized, then 96% ethanol and water are added and allowed to macerate 8 days. For its part, WO2005075614A1 summarizes the common characteristics of the extraction procedures of the compounds present in olive leaves: the leaf is usually dried and / or ground, extracted with an organic solvent, with water or with organic solvent mixtures / water, and in some cases Soxhlet extraction is used, finally the extract obtained is usually concentrated or dried by evaporation or lyophilization.
    However, effective procedures for extracting oleuropein from different parts of the olive tree are still needed.
    DESCRIPTION OF THE INVENTION
    The present invention relates to a process for obtaining oleuropein.
    The present invention has the following advantages:
    - it presents an effective method for the extraction of olive leaf oleuropein, therefore, it adds value to a raw material that does not have as much value as olives;
    - the use of pellets in the extraction makes the extraction of oleuropein more effective since it allows to obtain a greater amount of the compound;
    - The use of pellets also has the advantage that it makes handling and transporting the raw material easier; Y
    - Oleuropein obtained by the process of the invention has high purity.
    Therefore, a first aspect of the present invention relates to a process for obtaining oleuropein from olive leaves comprising the following steps:
    a) drying of olive leaves;
    b) pelletizing the dried leaves obtained in step (a); Y
    c) solid / liquid extraction of the pellets obtained in step (b) with a solvent selected from water, methanol, ethanol and any of their mixtures.
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    Surprisingly, it has been found that when the extraction is done on dry leaf pellets, more mg of oleuropelna is obtained per g of dry leaf than when the chopped leaf is used (see examples 1 and 2).
    Drying of olive leaves is known to any person skilled in the art. The leaves can be dried in air at room temperature, in the sun, or with blown air.
    By pelletizing in the context of the invention it is meant to form pellets, that is, small portions of agglomerated or compressed material. They are well known to a person skilled in the art. The pelletizing step (b) includes the cutting of the dried leaves until a suitable final particle size is reached and subsequent extrusion of the particles obtained using a piston or cylinder extruder at a high pressure, preferably between 5 bar and 25 bar. In this way a solid biomass (pellets) is obtained which is formed by very small cylinders, of a few millimeters in diameter.
    Solid-liquid extraction or leaching means the process of dissolving one or more components of a solid in a solvent.
    In an embodiment of the first aspect of the present invention, drying of step (a) is carried out in the air at room temperature.
    In another embodiment of the first aspect of the present invention, drying of step (a) is carried out with air between 20 ° C and 75 ° C, preferably drying of step (a) is carried out with air between 50 ° C and 70 ° C.
    In another embodiment of the first aspect of the present invention, the dried leaves obtained in step (a) have a water content of less than 10% by weight, preferably the dried leaves obtained in step (a) have a lower water content. at 5% by weight, more preferably between 0.5% and 5% by weight.
    In another embodiment of the first aspect of the present invention step (b) of pelletizing comprises a previous step (b1) of chopping. By cutting the dried leaf it is meant to cut the leaves in a knife chopper into smaller pieces (between 0.3 cm and 3.5 cm). Preferably, in step (b1) the chopping will be carried out until particles between 0.5 cm and 1.5 cm are obtained.
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    In another embodiment of the first aspect of the present invention, the pellets obtained in step (b) have a length less than 10 cm, preferably have a length between 3 cm and 6 cm.
    In another embodiment of the first aspect of the present invention, the pellets obtained in step (b) have a thickness of less than 15 mm, preferably have a thickness between 5 mm and 10 mm.
    In another embodiment of the first aspect of the present invention, the pellets obtained in step (b) have a length between 3 cm and 6 cm and are between 5 mm and 10 mm thick.
    In another embodiment of the first aspect of the present invention, the pellets obtained in step (b) have an apparent density between 0.30 g / cm3 and 0.60 g / cm3.
    In another embodiment of the first aspect of the present invention, the pellets obtained in step (b) have a length between 3 cm and 6 cm, have a thickness between 5 mm and 10 mm and have an apparent density between 0.30 g / cm3 and 0.60 g / cm3.
    In another embodiment of the first aspect of the present invention, the solid / liquid extraction of step (c) is carried out with ethanol, preferably with ethanol with a purity greater than 90% by volume, more preferably with ethanol with a higher purity 95% by volume. The extraction with ethanol favors the extraction of oleuropelna and minimizes the extraction of sugars.
    In another embodiment of the first aspect of the present invention, the solid / liquid extraction of step (c) is carried out at a temperature between 20 ° C and 95 ° C, preferably a temperature between 25 ° C is used in the extraction and 80 ° C.
    In another embodiment of the first aspect of the present invention, after the extraction stage (c) there is a filtration, preferably the filtration is carried out through a filter with a pore diameter between 0.45 pm and 0.20 pm .
    In another embodiment of the first aspect of the present invention, after the extraction stage (c) there is a stage (d) of adding water, preferably distilled. The addition
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    of water to the ethanol extract obtained in step (c) causes the precipitation of terpenes. Preferably, between 0.2 liters and 0.6 liters of water are added per liter of solvent used in step (c).
    In another embodiment of the first aspect of the present invention, after step (d) there is a filtration stage and / or a solvent evaporation stage. An evaporation of the partial solvent can be carried out, thus obtaining an extract of oleuropelna in solution or the extract can be taken to dryness, thus obtaining a powder.
    Throughout the description and the claims the word "comprises" and its variants are not intended to exclude other technical characteristics, additives, components or steps. For those skilled in the art, other objects, advantages and characteristics of the invention will be derived partly from the description and partly from the practice of the invention. The following examples are provided by way of illustration, and are not intended to be limiting of the present invention.
    EXAMPLES
    The invention will be illustrated below by tests carried out by the inventors, which shows the effectiveness of the product of the invention.
    Example 1. Procedure for extracting oleuropelna.
    2 kg of olive leaves were air dried for a week, extended without exceeding a height of 60 cm until the water content was less than 5%.
    The dried leaves were chopped (sieve-0.50 mm) and pelletized with a manual flat die pelletizer using a piston extruder at a pressure of 10 bar. In this way, pellets formed by cylinders 6 mm in diameter and 4 cm in length were obtained; bulk density of 0.46 g / cm3.
    1 kg of pellets were extracted with 25 liters of 96% ethanol, in Soxhlet at reflux. Extraction time of 3 h and number of siphonations 4.
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    After extraction, the pellets of the ethanol extract were removed by passing the extract through a Miracloth filter (filter cloth). The concentration of oleuropein in the ethanol extract was 4.2 mg / mL with a purity of 56%.
    To the filtrate 10 liters of distilled water were added and the mixture was passed through a 0.45 pm filter.
    The extract was concentrated by vacuum distillation (T <40 ° C) until reaching a volume of 5 liters. The aqueous concentrate had an oleuropein concentration of 20.1 mg / mL with a purity of 71%.
    Example 2. Comparative example of extraction of oleuropein (without pelletizing stage)
    2 kg of olive leaves were dried with an air flow of 0.7 m / s, at 50 ° C for 10 hours, resulting in the water content of the dry leaf less than 5%.
    The dried leaves were chopped into pieces of a size smaller than 0.5 cm.
    1 kg of dried leaf was extracted with 25 liters of 96% ethanol, in Soxhlet at reflux. 3 h extraction time and number of siphonations 4.
    The extracted leaf was removed from the ethanol extract by passing the extract through a Miracloth filter. The concentration of oleuropein in the ethanol extract was 3.6 mg / mL and its purity was 60%.
    To the filtrate 10 liters of distilled water were added and the mixture was passed through a 0.45 pm filter.
    The extract was concentrated by vacuum distillation (T <40 ° C) until reaching a volume of 5 liters. The aqueous concentrate as! obtained I present an oleuropein concentration of 17.6 mg / mL with a purity of 73%.
    权利要求:
    Claims (18)
    [1]
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    1. Procedure for obtaining oleuropelna from olive leaves comprising the following stages:
    a) drying of olive leaves;
    b) pelletizing the dried leaves obtained in step (a); Y
    c) solid / liquid extraction of the pellets obtained in step (b) with a solvent selected from water, methanol, ethanol and any of their mixtures.
    [2]
    2. Method according to claim 1, wherein the drying of step (a) is carried out with air between 20 ° C and 75 ° C.
    [3]
    3. Method according to claim 2, wherein the drying of step (a) is carried out with air between 50 ° C and 70 ° C.
    [4]
    4. The method according to any of claims 1 to 3, wherein the dried leaves obtained in step (a) have a water content of less than 10% by weight.
    [5]
    5. Method according to claim 4, wherein the dried leaves obtained in step (a) have a water content of less than 5%.
    [6]
    6. Method according to any one of claims 1 to 5, wherein the pelletizing step (b) comprises a previous step (b1) of chopping.
    [7]
    7. Method according to any of claims 1 to 6, wherein the pellets obtained in step (b) are less than 10 cm long.
    [8]
    8. Method according to claim 7, wherein the pellets obtained in step (b) have a length between 3 cm and 6 cm.
    [9]
    9. Method according to any of claims 1 to 8, wherein the pellets obtained in step (b) are less than 15 mm thick.
    [10]
    10. Method according to claim 9, wherein the pellets obtained in step (b) have a thickness between 5 mm and 10 mm.
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    [11]
    11. Method according to any of claims 1 to 10, wherein the pellets obtained in step (b) have an apparent density between 0.30 g / cm3 and 0.60 g / cm3.
    [12]
    12. Method according to any of claims 1 to 11, wherein the
    solid / liquid extraction from step (c) is carried out with ethanol.
    [13]
    13. Method according to any of claims 1 to 12, wherein the
    solid / liquid extraction from step (c) is carried out with ethanol with a purity greater than 90% by volume.
    [14]
    14. Method according to any of claims 1 to 13, wherein the
    solid / liquid extraction from step (c) is carried out at a temperature between 20 ° C
    and 95 ° C.
    [15]
    15. Method according to any one of claims 1 to 14, wherein after the extraction step (c) there is a filtration.
    [16]
    16. The method according to any one of claims 1 to 14, wherein after the extraction stage (c) there is a stage (d) for adding water.
    [17]
    17. Method according to claim 16, wherein between 0.2 liters and 0.6 liters of water are added for each liter of solvent used in step (c).
    [18]
    18. Method according to any of claims 16 or 17, wherein after step (d) there is a filtration stage and / or a solvent evaporation stage.
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    同族专利:
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    ES2631004R1|2017-08-29|
    ES2631004B1|2018-06-08|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    ES2804376A1|2019-08-05|2021-02-05|Roque Iniciativas Sl|PROCEDURE FOR OBTAINING A FOOD SUPPLEMENT DERIVED FROM THE OLIVE TREE PLANT AND FOOD SUPPLEMENT OBTAINED |
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