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    • 专利摘要:
    A pleasant taste and smell syrup containing carbohydrates, micronutrients and refined water soluble polyphenols of the carob bean pod and process for obtaining them. The syrup comprises 20-55% sucrose, 5-20% glucose, 2-18% fructose, 0.3-5% other sugars, 6-19% cyclitol (mainly D-Pinitol), 0.4-3.5% potassium, 0.35-4% refined phenolic compounds and 0.3-8% organic and inorganic impurities. The process includes the aqueous extraction of the water soluble components present in the pod of the carob, the purification by ultrafiltration by membranes, and the refining with adsorbing agents, in order to separate the desired components from those that are not. The field of application of the obtained syrup is equal to that of other sugars and natural sugar syrups. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2641963A1
    申请号:ES201731000
    申请日:2017-08-01
    公开日:2017-11-14
    发明作者:Gregorio MARTINEZ-FORTUN PEREZ；Jose Ignacio LOPEZ SANCHEZ；Jose Maria MARTINEZ-FORTUN HERNANDEZ
    申请人:Gregorio Martinez-Fortun S L；Gregorio Martinez-Fortun Sl；
    IPC主号:
    专利说明:

    NICE TASTE AND ODOR SYRUP CONTAINING CARBOHYDRATES, MICRONUTRIENTS, AND NATURAL REFINED POLYPHENOLS OF ALGARROBA, AND METHOD FOR OBTAINING IT.
    SECTOR OF THE TECHNIQUE
    C13B 20/00; Purilication 01 sugar juices [2011.01]
    C13B 20/16; By physical means, e.g. osmosis or liltration [2011.01]
    C13B 12/20; Using adsorption agents, e.g. active carbon [2011.01]
    BACKGROUND OF THE INVENTION
    Carob has been applied as a food product since ancient times. In fact, the existence of carob syrups that are mainly marketed in Mediterranean countries is known, such as Italy, Morocco, Portugal and even Spain, among others, in the form of carob syrups. However, these correspond to the result of evaporating water on the first aqueous extract of the unpurified locust bean pod, containing a mixture of all the water-soluble elements that exist in the locust bean pod, resulting in compositions with a strong dark color , which, although sweet in taste due to their high sugar content, maintain harsh tones of unpleasant taste and smell characteristic of carob, as described previously in the state of the art (see for example the patent ES2060544A 1 and the documents cited in her).
    In addition, in the state of the art a solution for the
    use of natural sugars from carob, by means of
    Obtaining a colorless and odorless syrup that contains the sugars from the carob tree naturally (this syrup and its obtaining are
    described in patent ES2060544A1). However, this solution has
    important disadvantages:
    a) On the one hand, it dramatically reduces the micronutrient content
    (demineralized) and polyphenolic compounds of the product, decreasing
    5 so dramatically, as we will reason in-extense later, the nutritional properties of the product with respect to which the carob tree possesses
    naturally or the previously mentioned raw carob syrup (In !. J. Food Sci. Nutr., 2007, vol. 58 (8), 652-658; In !. J. Mol. Sci. 2016, 17 (11 ), 1875 (1-20)).
    10 b) On the other hand, it complicates the process of obtaining said sugar syrup in such a way that it is not very efficient and has a high environmental impact (as described in the state of the art, for example in
    patent ES2284381A1), making it less competitive compared to other sugars.
    This is mainly because of the bleaching and demineralized processes proposed in the mentioned solution (ES2060544A 1)
    It is necessary to use ion exchange resins, which must be regenerated with acidic, basic and / or high mineral salt solutions (brines), generating residues (dirty brines) of
    Difficult management and very polluting. Although a possible one has been proposed
    20 technical solution to this problem by using a step of extracting in supercritical fluids of carob carbohydrates (see
    Patent ES2284381A 1), it is not exempt from serious limitations that make it difficult to transfer on an industrial scale, related to complex and
    expensive facilities required for working with fluids in supercritical conditions, such as high pressures, high temperatures, high
    safety requirements and very high production costs (see for example: RSEQ Annals, October-December 2003, No. 4, 15-23). Although the use of supercritical fluids in the pharmaceutical and food industries has increased in recent years, it remains limited to products of very high
    30 high added value for the reasons mentioned, a condition a priori not satisfied by sugars or sugar syrups, which are usually aimed at large volume markets where there is high competition
    between products of different origin.
    The use of carob dates back to ancient Egypt, who collected their fruits for cattle, among other uses. The seed has also been used 5 as a unit of weight by Arab peoples, who
    called "karat", taking it as a standard of weight against gold and stones
    Precious (see for example, Compro Rev. Food Sci. Food Sal. 2016, 15 (1), 63
    72) In addition, since its inception the fruit of the carob tree has been used as food, largely due to its high content of
    10 sugars However, at present, their employment is mostly limited
    to the seed, which represents only 110% of the weight of the fruit, from which
    LBG (E410), used as a thickener, yaromatizing stabilizer, is extracted
    in food, pharmaceutical and cosmetic industries mainly. The rest of the fruit, the pod, representing 90% by weight, is used ha
    15 has been used until now mainly as a by-product for animal feed. However, this is changing recently since the pod of the carob fruit is rich in a wide range of compounds of high nutritional value and healthy bioactive properties, especially its content in bioactive polyphenols, and also in cycitols (mainly D
    20 Pinitol) and mineral salts (see, for example, high-impact and high-impact scientific reviews such as: Inl. J. Food Sci. Nutr., 2007, vol. 58 (8), 652658; InL J. Mol. Sci. 2016 , 17 (11), 1875 (1-20 ». Because of this, a number
    Important researchers have recently recommended the inclusion of this product in the diet, claiming about the beneficial properties it provides, such as diabetes control, prevention of heart problems, the lower frequency of certain types of cancer, or their
    anti-inflammatory properties, among others ((lnL J. Food Sci. Nutr., 2007, vol. 58 (8), 652-658; InL J. Mol. Sci. 2016, 17 (11), 1875 (1-20 "That is why the
    Object of the present invention is focused on obtaining a syrup
    30 sugary carob with high added value, which on the one hand has a smell,
    pleasant color and taste, but which in turn respects the nutritional qualities and
    healthy that the product presents at its origin, a problem that up to 4
    Present invention was unsolved.
    Additionally, the use of the carob pod to obtain value-added products such as the one presented here, has
    predictably a positive impact by stimulating crop creation of
    5 carob trees, which have been shown to have a lower carbon footprint than other crops when performing the life cycle and carbon footprint analysis (see
    Chem. Eng. Trans. 2010, 21,613-618).
    In the scientific literature it has been found that ultrafiltration by membranes has potential application in process improvement
    10 traditional cane sugar purification (See for example the following reference: Sep. Pur. Technol. 2001, Vol. 21 (3), 247-259), and also in the separation of carbohydrates and polyphenols from certain fruit juices (reference Inter. Scholar. Sci. Res. Innovation 2007, vol 1 (10), 115-122). However, we have not found any reference on its application to the purification of
    15 sugary carob syrups. Surprisingly, in the course of
    our investigations found that by means of an ultrafiltration operation on membranes it was possible to purify the juice from the aqueous extraction of the water-soluble compounds of the carob pod, sugars, cyclosols (mostly D-Pinitol), micronutrients and 20 refined polyphenols, from such that they are separated simply and very
    efficient of unwanted compounds that would give it black color, and taste and
    unpleasant odor, allowing obtaining a syrup of pleasant taste and smell, which contains carbohydrates, micronutrients and refined water-soluble polyphenols
    25 natural carob pod.
    EXPLANATION OF THE INVENTION
    This invention relates to a syrup of pleasant taste and smell, which contains carbohydrates, micronutrients and water-soluble polyphenols.
    30 natural refined carob pod and with a process to obtain it. The syrup object of the present invention is obtained by means of a
    aqueous extraction process of carob pulp, and subsequent application
    of physical refining methods, specifically ultrafiltration and neutral adsorbents, avoiding the strong cationic resins described in the state
    of art (ES2060544A1), bleached ion exchange columns and
    demineralizers, since these drastically reduce the nutritional qualities of the product, raise its production cost and generate significant
    waste, so that with the process of the present invention the syrup obtained finally contains the minerals and water-soluble carbohydrates of the
    carob pulp and also an important part of the polyphenolic compounds that as we have said before are healthy, but nevertheless our syrup is free of those other compounds that
    give traditional carob syrups some properties
    negative organoleptics, such as an intense black color, as well as unpleasant smell and taste.
    The fields of application of the product provided herein
    invention should be contemplated in those uses similar to those of other sugars and sugary syrups, including colorless sugary syrups and
    toilets from the carob bean described in the state of the art, but with
    the following benefits: i) Lower production cost than known sugary syrups, including lower production cost than syrups
    colorless and odorless locust beans (approximately 40% lower than the latter); ii) Lower environmental impact on its production than
    known sugary syrups, including colorless and odorless carob sugar syrups (approximately 50% lower energy consumption and 45% lower water, compared to the latter) ii) Properties
    Organoleptics suitable for more extensive use than traditional black carob syrup and unpleasant taste and smell and iii)
    Better nutritional characteristics than the colorless and odorless carob sugar syrups described in the state of the art, due to their content in micronutrients and refined polyphenols.
    To obtain this product, a colored carob syrup,
    pleasant taste and smell, which contains carbohydrates, micronutrients and
    Natural refined water-soluble polyphenols from the carob pod, se
    They carried out a series of research works aimed at obtaining a natural carob extract in which the negative characteristics of the juice, such as its intense black color, as well as its smell and taste, had been removed simply and effectively by physical methods excessively intense and bitter,
    but, in contrast to the state of the art (ES2060544A 1), that this is
    carried out selectively, so that not only carbohydrates and cyclitols (mainly O-Pinitol), but also micronutrients (eg mineral salts, remain in the syrup, since the carob pod is very rich in, for example potassium that has important functions at the muscular level and the
    nervous system), and a part of water-soluble polyphenols, for their proven health benefits (see for example Inl. J. Food Sci. Nutr., 2007, vol. 58 (8), 652-658; Inl. J. Mol. Sc ;, 2016.17 (11), 1875 (1-20)). For it,
    new techniques were investigated, such as ultrafiltration with membranes,
    that allow discriminating between permeate (obtained broth) and rejection (broth
    surplus) by range of molecular sizes, and the use of adsorbent agents, avoiding in any case the cationic resins and demineralizers described
    in the state of the art since they entail the inconveniences of a high cost
    of production and of an important generation of waste with high environmental impact.
    In order to obtain the product according to this invention with the aforementioned properties, the problem to be solved was focused on achieving a technically feasible process that would allow, in a cost-effective, efficient and environmentally friendly manner, to obtain the sugars, cyclosols (mainly D-Pinitol), micronutrients and healthy polyphenols that carob naturally possesses, but in such a way that the syrup obtained had adequate organoleptic and nutritional qualities, that is, that it had a pleasant taste and smell and a commercially acceptable color, not intense black, at the same time. that, as we have said, there would not be a drastic decrease in its beneficial qualities for health with respect to the original raw material, which has great nutritional benefits that it is important to preserve. Therefore, all research and development efforts focused on these points.
    With respect to the extraction phase of organic compounds
    water-soluble and mineral salts, it is known that the pulp of carob 5 is formed by a multitude of cells delimited by a cell wall
    permeable to dissolved substances, but that, however, there is also an ectoplasmic membrane which, before ripening the fruit, seems to be only permeable to water, but not to dissolved substances. It is also known that in the dried fruit, said ectoplasmic membrane loses that
    10 property, allowing the passage of certain water-soluble molecules, such as
    the sugars
    In the course of our investigations we discovered that, like carbohydrates, the mineral salts of interest (micronutrients), as well
    like the healthy water-soluble polyphenols that we want to extract and
    15 preserved in the syrup, they are extractable from the carob pod with water at normal temperatures, making temperature rise unnecessary, which is an advantage over obtaining sugars from other natural sources, such as beets (see for example the information contained in ES2060544A 1 and the documents cited therein).
    20 With respect to the purification of the must, or juice resulting from the
    aqueous extraction of carob pulp, there is a wide variety of
    agents and procedures described in the state of the art for the stages of
    coarse filtration, fine filtration, clarified, discolored and deodorized, such as purification with whitewash, lime and alumina, bentonites, activated carbon, 25 exchange and demineralizing resins or combination of the above. However, none of them alone or in combination, provides the desired product, a carob syrup of adequate color for
    food industry, not black, and pleasant taste and smell, which contains
    not only carbohydrates, but also natural refined micronutrients and water-soluble polyphenols 30 from the carob pod.
    After continuing with our investigations, it was surprisingly proven that the purification of the juice of the first extraction by using ultrafiltration by membranes, gave excellent results in the separation of those organic and inorganic species that were desired (carbohydrates, cyclyols such as D -Pinitol, micronutrients and refined water-soluble polyphenols) selectively with respect to that other important part of unwanted organic species, which were mostly responsible for the negative organoleptic properties. Surprisingly, it was also discovered that this permeated juice of ultrafiltration in membranes, could be further refined in its organoleptic qualities, until obtaining more palatable tones of flavor and smell, through a simple and very efficient operation of passage through a column filled with an agent adsorbent, without loss in its nutritional properties. Although the application of these neutral adsorbent agents has been reported in the state of the art as very disadvantageous, due to their high inefficiency, when used on juice from the crude aqueous extract of carob (see the information contained in patent ES2060544A1), we discover unexpectedly, when some of these adsorbents were applied to the previously ultrafiltered juice, they greatly increased their effectiveness, and furthermore, their subsequent regeneration could be carried out simply and efficiently, by means of environmentally friendly processes, with virtually no waste generation. Among the adsorbent agents tested successfully are active carbon and neutral adsorbent resins (non-cationic, anionic, or demineralizing), which, as said, were greatly increased by receiving the juice after the ultrafiltration operation on membranes, with respect to the inefficient results obtained by passing the non-ultrafiltered juice.
    Specifically, according to the present invention, the purification of the juice, resulting from the aqueous extract of the carob bean pod, by ultrafiltration by membranes and subsequent contact with an adsorbent agent, was carried out as follows:
    The prefiltered juice (coarse filtration) is conducted to a membrane ultrafiltration equipment, consisting of: i) two tanks, one inlet and
    reception of the recirculated juice, and another of the output of the permeated juice, ii) a passage through membranes where ultrafiltration takes place and iii) a pump that keeps the juice in recirculation as well as adequate pressure and flow rates.
    Surprisingly, the membranes used for a molecular level separation of the compounds of interest, from those other compounds not
    desired, are those of pore sizes in the range of 1 KDalton (1000 dalton) to 150 KDalton, more specifically those of around 1, 5, 8, 15, 50 and 150 KDalton, obtaining the best results with the membrane of size
    Pore of 1 KDalton or less. This stage of membrane ultrafiltration is a process of continuous purification, since the volume at the exit of permeated and purified juice is replaced in the inlet tank with virgin juice of the first extraction.
    After membrane ultrafiltration, the juice obtained has a color
    yellow orange. This product can be concentrated (evaporate water) until
    the desired Srix grades, preferably between 65-75 Srix, obtaining an appetizing honey-colored syrup, of pleasant organoleptic qualities, since
    its smell and taste have been considerably improved compared to
    Starting juice that would give rise to syrup or traditional carob syrup.
    Moreover, the treatment with adsorbent agents of the juice obtained after
    The ultrafiltration operation on membranes, such as activated carbon or non-cationic, anionic or demineralizing adsorbent resins, results in an even more refined product, with softer color, smell and taste tones. Surprisingly, in our investigations we discovered that the adsorbent agents used greatly increased their effectiveness and acting capacity, when used on ultrafiltered membrane juice, with
    regarding its use on non-ultrafiltered juice, with refining capacities for juice volumes between 10 and 50 higher according to the present
    invention. Thus, in our invention the use of this type of
    adsorbent agents, which is not recommended in the state of the art for the
    processed of sugary carob syrups, becomes an operation
    recommended after ultrafiltration, as it is efficient (allows treatment
    of large volumes of juice), economically viable (1050 times less adsorbent agent is needed than without previous ultrafiltration and also
    this agent becomes easily regenerable) and environmentally
    Respectful (waste generated by regeneration of adsorbents is
    practically null). Elio, as described herein
    invention, performing a membrane ultrafiltration operation prior to the use of adsorbent agents. The adsorbent agents used with satisfactory results were: activated carbon, bentonites, as well as neutral adsorbent resins, which further improve the process significantly with respect to the ionic resins used in the state of the art
    (ES2060544A1). Thus, we use with good results among other resins
    neutral, the following: polystyrene resins, polystyrene resins crosslinked with divinylbenzene, acrylic resins and cyclodextrin-based resins. The best results were obtained by using as an adsorbent activated carbon, both powder and granular.
    Specifically, the ultrafiltered membrane juice is passed through a column filled with granular activated carbon of vegetable origin based on coconut bark. During the passage of the juice a part of the dye molecules that have survived the passage through ultrafiltration accompanying carbohydrates and minerals, are stopped by partial adsorption on the surface of the adsorbent agent, in this case activated carbon, due to weak electrostatic interactions of Van-der-Waals type. However, carbohydrates and micronutrients, of great affinity for the liquid (aqueous) phase, pass through the column without being retained. As a consequence, the juice at the exit has a smaller load of those coloring molecules that are also those that still give it a certain, although low already, bitter hue to carob. The advantage of using neutral adsorbent agents such as those discussed in the present invention (active carbon, bentonites or neutral resins), is that the adsorption of the dye molecules is weak and therefore, the adsorbent agent can be easily regenerated by reversing the process, that is, causing desorption with hot water or hydroalcoholic mixtures, without the use of brines, or acid solutions
    or basic high cost and environmental impact, which would be the case in ionic and demineralizing resins.
    5 The syrup thus obtained, after concentrating by evaporating water to the desired Brix degrees, is a natural, honey-colored, honey-colored carob syrup
    and pleasant taste, containing carbohydrates (sucrose, glucose and fructose),
    cycitols (mainly O-Pinitol), micronutrients (eg high content in
    potassium), and healthy refined polyphenols, which has the following 10 advantages compared to existing syrups from carob:
    1) On the raw carob syrup:
    Elimination of the intense black color, and the unpleasant taste and smell characteristics that hinder its commercialization as sugary syrup.
    2) On the totally colorless and demineralized carob syrup
    15 described in the state of the art (ES2060544A 1):
    Better nutritional properties and healthy properties, for its
    contribution in essential micronutrients such as potassium and its content in refined polyphenols. Lower cost and lower environmental impact on its production.
    Therefore, and according to a first aspect, the present invention provides a natural carob syrup consisting of the following components:
    Sucrose: 20-55%
    Glucose: 5-20%
    25 Fructose: 2-18%
    Other sugars: 0.3-5%
    Cyclitols (mainly O-Pinitol): 6-19%
    Potassium: 0.4-3.5%
    Phenolic compound (flavonoids, glycosylated flavanols and hydrolysable tannins): 0.35-4%
    5 Organic and inorganic impurities: 0.3-8%
    Where the percentages are expressed in weight of the dry matter and the intervals given in such a way that the possible logical variations due to the particular origin of each fruit, such as its variety, the parameters that affect the harvest (rains,
    10 terrain, etc.), among others.
    Additionally, and according to a second aspect of the invention, there is provided a method for obtaining the
    Natural carob extract of the above-mentioned composition, which encompasses the following stages:
    15 1. Carob cleaning.
    2. Chopped thick.
    3. Sheath and seed separation.
    Four. Thin chopped
    5. Aqueous extraction of water-soluble components of the
    20 pod
    6. Pressing.
    7. Coarse filtering.
    8. Ultrafiltration in membranes.
    9. Treatment with an adsorbent agent.
    10. Concentration BRIEF DESCRIPTION OF THE DRAWINGS
    PROCESS DIAGRAM.5 Figure 1. Diagram of the constituent stages of the process.
    ILLMPIEZA DE LA ALGARROB! Il7 ttROCEADO GRUESq 7
    7 1 SHEEP AND SEED SEPARATIONj7 ttROCEADO FINOl7
    7 1 EXTRACCION ACUOS! Il7 IPRENSADq 7 1FIL TRADO GRUESq 7
    7 1 MEMBRANE TRAFFICKING § 7
    10 7 tTREATMENT WITH AN ADSORBENT AGENT j7 ICONCENTRACIONI
    PREFERRED EMBODIMENT OF THE INVENTION
    1. Carob cleaning.
    The carob fruit comes from the field, so it comes
    5 generally accompanied by a series of strange elements, foreign to the fruit such as earth, stones, branches or possible metallic elements, among others. Therefore, the first operation to be carried out is the cleaning of all these elements outside the carob fruit, in order to obtain a clean fruit, allowing the entry into the chopping phase under adequate conditions of
    10 hygiene. This cleaning is carried out both manually and mechanically in the case of metal objects.
    2. Thick chopping.
    The cutting is carried out in a hammer mill, adjusted to break the sheath into pieces of adequate size, without damaging as far as possible the seed garrotín, which separates intact from the pod. In this way, an excessively thick cut locust bean pod is obtained for aqueous extraction (diameter around 2 cm). This diameter is excessive for extraction since thicker sizes require longer extraction times for water to penetrate inside the sheath and
    20 soluble products are diffused in the aqueous phase. However, a thinning of the finest pod is not possible at this point since this would cause the seed to break, compromising its use.
    As for the operating conditions, it is necessary to avoid heating at this stage by friction that can lead to a temperature rise and degradation of sugars. Thus, the temperature is controlled
    at all times to be below 40 oC.
    3. Separation of pod and seed.
    The product obtained after the previous stage of coarse cutting, is going to
    stop a sieve that separates the seed from the thick sheath pieces. This sieve acts automatically by a spring vibration system driven by a low consumption motor.
    4. Thin slicing.
    5 The thick sheath pieces are taken to a new cutting hammerNow, crush them to the right size for proper operationextraction (approximately 0.5 centimeters in diameter). Crushedexcessive generates a large number of fines that subsequently complicatefiltering processes Therefore, the size of the chopper is adjusted to a
    10 compromise situation, in which the extraction times are not too long, but the amount of fines produced is not excessive.
    As in thick chopping, in terms of operating conditions it is necessary to avoid friction heating, controlling everything
    moment the temperature does not exceed 40 oC.
    15 5. Aqueous extraction of the water-soluble components of the sheath.
    The extraction is carried out in a discontinuous reactor, with a ratio between chopped pod and water of between 1.3 and 3 liters of water per kilogram of chopped pod. Contact times with good agitation are low, around 30-45 minutes, insufficient for the proliferation of
    20 microorganisms, avoiding unwanted fermentation and other processes
    Biological anomalies. The temperature for extraction is between 15 and 35
    oC.
    6. Pressing.
    Taking into account that the carob pod has a high tendency to
    25 absorb moisture, with the capacity to retain around its weight in water, and that the process performance depends largely on the effectiveness of this stage of separation of the juice from the residual organic vegetable matter, it is clear that it is essential to use a pressing method as efficient as possible.
    In the course of our investigations, continuous and discontinuous industrial pressing methods were tested, obtaining satisfactory results with roller and piston presses, with the difference that the first works in continuous and the second in discontinuous.
    5 The temperature for this pressing operation is between 15 and35 oC and times depend significantly on the type of pressemployee.
    7. Coarse filtering.
    The juice obtained after the pressing operation drags a quantity
    10 important solids of varied sizes. These have to be removed before moving on to the next stage of ultrafiltration by membranes, since otherwise they would cause significant problems.
    In the course of our investigations we discovered that it is essential that coarse filtration be carried out sequentially, until
    15 degree of final fineness required. That is to say, a series of sieves of increasingly thinner thickness have to be used, since if only the finest sieve screen is used, the broth obtained will have the same quality, but the filter will suffer from repeated obstructions that will make it impracticable the operation fluidly.
    20 After several tests, we found that an effective sieve sequence that allows continuous work in a fluid manner, includes filtering at approximately 300, 100 and 40 microns. In addition, in the market there are varied solutions that allow the mechanical cleaning of the sieves continuously, without the production having to stop at logical working times.
    25 The juice thus obtained still has an important load of suspended solids smaller than 40 microns in size, although this is much lower than the initial one, and does not pose a serious problem for the next stage of membrane ultrafiltration, since it is not capable of obstructing the ducts in the membranes, which have a much larger diameter, and also do not involve
    limiting decrease in the fluidity of the juice, which must be continuously
    recirculating by the action of a bomb. However, the final syrup must be
    free of suspended particles and therefore, in order to determine the nature and proportions of them and thus refine in their withdrawal after this operation of
    coarse filtering, we carry out a particle size analysis by
    light scattering methods, finding that they are in approximate proportions between 2-7%, with sizes always greater than 0.1 microns.
    8. Ultrafiltration in membranes.
    The juice obtained after the coarse filtration operation is taken to the entrance tank to the ultrafiltration equipment by membranes. At this point the juice contains, on the one hand, suspended particles of less than 40
    microns and not greater than 0.1 microns, and on the other hand, dissolved species, organic (carbohydrates, cyclites such as O-Pinitol and polyphenols mainly), and inorganic (including potassium, magnesium and calcium ions). This juice can be concentrated, where a traditional carob sugar syrup (sweetened by its high sugar content), black color, taste and smell would be obtained
    Very intense carob. However, that product has limited applications as has been explained extensively before. Additionally, as we have discussed above, this juice can be subjected to bleaching and demineralized operations using ion exchange and demineralizing queens, to obtain a completely colorless sugar syrup, with a fruity sweet taste and smell, as described in the state of art (ES2060544A1). However, the process for this, as has already been reasoned, is expensive, has a high environmental impact and results in a
    product that has lost an important part of its properties
    Nutritional, since it is completely exempt from the minerals provided by the
    carob, some of them of great importance as potassium, and is also exempt from all the healthy polyphenols that carob contains in its
    origin, backed by recent scientific studies of the highest level (see for
    example In !. J. Food ScL Nutr., 2007, vol. 58 (8), 652-658; In !. J. Mol. ScL 2016, 17 (11), 1875 (1-20)). Our goal was to find a method of
    Purification of the juice that allowed discriminating between those unwanted molecular components that infer the product some negative properties of color, smell and taste, which we therefore wanted to remove, and those other molecular components of the juice that without negatively affecting its organoleptic properties, provide nutritional and healthy properties
    Carob beans.
    Through the ultrafiltration operation by membranes, first of all a juice that is completely clarified is achieved, that is to say absent from
    suspended particles. In addition, a juice that is no longer black, but has
    a yellow-orange color, once concentrated similar to honey.
    Additionally, the juice obtained has greatly reduced the taste and smell tones
    carob characteristics that they don't like, being much softer. Surprisingly, the thorough chemical analysis of this juice indicated that,
    In addition to carbohydrates and cyclites, it still contains a large portion of
    Polyphenolic compounds of healthy properties.
    Preferably, the membrane ultrafiltration equipment consists of an inlet and receiving reservoir of recirculated juice, an outlet tank of the permeated juice through the membrane, and a pore-sized 1000 dalton (1KDalton) membrane passage. The operation is performed in a way
    continue, so that the volume of permeated juice is replenished with
    Virgin juice in the entrance tank. The working temperature is between 30-40 oC, so that, without degrading the sugars or the rest of the
    components dissolved in the water, the fluidity is maximum and with it the permeate flow.
    After this membrane ultrafiltration operation, the juice obtained has a yellow-orange color. This product can be concentrated.
    (evaporate water) to the desired Brix degrees, preferably between 65-75 Brix, obtaining an appetizing honey-colored syrup, of qualities
    Pleasant organoleptics, since their smell and taste have been greatly improved
    with respect to the starting juice that would give rise to the syrup or traditional syrup of
    carob.
    9. Treatment with an adsorbent agent.
    Treatment with certain neutral adsorbent agents (not cationic, anionic or demineralizing resins), of the juice obtained after the ultrafiltration operation 5 in membranes, results in an even more refined product, with
    shades of color, smell and taste still softer and appetizing.
    Surprisingly, the adsorbent agents employed have very high efficiencies and the ability to treat very large juice volume ratios.
    Treated (Ljugo) against adsorbent weight (Kg.adsorbent): 10 Ljugo / Kg.adsorbent. This relationship is much more favorable now, okay
    to the present invention, which was with the non-ultrafiltered juice, obtaining
    ratios even of Ljugo / Kg.adsorbent = 100 L / Kg, when
    proven that the non-ultrafiltered juice saturates the same adsorbent agents
    with ratios even less than 10 L / Kg. Surprisingly, the juice 15 treated retains an important part of the nutritional properties and
    healthy that carob has in its origin.
    Preferably, the juice obtained after the ultrafiltration operation in
    1 KDalton membrane was passed through a column filled with
    granular active carbon of vegetable origin based on coconut bark,
    20 process in which all carbohydrates, cyclitols (mostly D
    Pinitol) and minerals pass without being retained, as well as an important part of
    polyphenols, flavonoids, glycosylated flavanols and hydrolysable tannins, while
    that the part of the dye molecules with the worst taste and smell that still
    remained are braked by partial adsorption on the surface of the agent
    25 adsorbent, due to weak electrostatic interactions of the Van-der-Waals type.
    This surprising preferential affinity can be attributed to the particular chemical nature of the worst tasting and odor coloring substances present in carob, characterized by the presence in its structure of aromatic rings, as well as phenolic groups and carboxylic groups, all capable of interact with the adsorbent as we have commented. Therefore, the juice
    Brilliant gold, which once concentrated up to 65-75 Brix gives rise to a golden syrup very pleasant to the palate, the pot and the view.
    The operation is carried out at a temperature between 25-35 oC,adjusting the flow through the column in such a way that the times of5 contact between the juice and the adsorbent agent are appropriate, according
    to the manufacturer's recommendations (each neutral adsorbent agent of the
    employees have theirs).
    10. Concentration
    The juice from the previous stages of ultrafiltration and treatment with 10 neutral adsorbents, which is between 24-27 Brix, must
    concentrate, evaporating water, up to 65-75 Brix, which are the appropriate values for commercialization. This operation has to be carried out avoiding that the juice suffers from intense thermal stress, taking care that the
    temperatures do not exceed 55-60 oC for as short a time as possible.
    15 In the market there are many industrial solutions for this purpose, being the one we have used in the course of our investigations,
    a vacuum concentrator of the descending film type.
    DOCUMENTS CITED
    1. Nasar-Abbas, S. M .; Zill-e-Huma; Vu, T-H .; Khan, M. K .; Esbenshade,
    20 H .; Jayasena, V. "Carob Kibble: A Bioactive-Rich Food Ingredienf '. Compr. Rev. Food Sci. Food Saf 2016, 15 (1), 63-72.
    2. ES2060544A 1 (Cia. Gral. Del Algarrobo de España, SAl and the
    documents cited therein.
    3. ES2284381A1 (Cia. Gral. Del Algarrobo de España, SAl and the 25 documents cited therein.
    4. Qzcan, M. M .; Arslan, D .; Gbk, alik, H. "Some compositional properties and mineral contents 01 carob (Ceratonia siliqua) lruit, Ilour and syrup". Inl. J. Food Sci. Nutr., 2007, vol. 58 (8), 652-658.
    5. Goulas, V .; Evgenios Stylos, E .; Chatziathanasiadou, M. V .; Mavromoustakos, T .; Tzakos, A. G. "Functional Components 01 Carob Fruit: Linking the Chemical and Biological Space". Int. J. Mol. Sci. 2016, 17 (11), 1875 (1-20)
    5 6. Sanchez Segado S., Lozano L. J., by Juan Garcia D., Godinez Seoane C., de los Rios A. P., Hernandez Fernandez F. J. "Lile Cycle Assessment Analysis 01 Ethanol Production Irom Ca rob Pod." Chem. Eng. Trans. 2010, 21, 613-618
    7. Bhattacharya, P. K .; Agarwal, S .; Gopal, R. "Ultraliltration 01 sugar cane
    10 juice for recovery of sugar: analysis of flux and retention "Sep. Puro
    Technol 2001, Vol. 21 (3), 247-259.
    8. Wei, D. S .; Hossain, M .; Saleh, Z. S. "Separation 01 Polyphenolics and Sugar by Ultraliltration: Effects 01 Operating Conditions on Fouling and Dialiltration" Inter. Scholar Sci. Res. Innovation 2007, vol 1 (10), 115
    15 122.
    9. Sotelo-Sancho, J. L .; Ovejero-Escudero, G. "Processes with supercritical fluids" Anales RSEQ, October-December 2003, N ° 4, 15-23
    权利要求:
    Claims (3)
    [1]
    1. A pleasant taste and smell syrup, which contains carbohydrates,
    micronutrients and natural refined water-soluble polyphenols of the pod
    5 carob, more specifically constituted by the following components:Sucrose: 20-55%Glucose: 5-20%
    Fructose: 2-18%Other sugars: 0.3-5%
    10 Cyclitols (mainly O-Pinitol): 6-19%
    Potassium: 0.4-3.5%Phenolic compound (flavonoids, glycosylated flavanols and tannins
    hydrolysable): 0.35-4%
    Organic and inorganic impurities: 0.3-8%
    15 2. A process for obtaining the syrup of pleasant taste and smell, the
    which contains carbohydrates, micronutrients and water-soluble polyphenols
    Natural refining of the carob pod according to claim 1, characterized in that it comprises the following steps:
    a) Carob cleaning, as the carob tree when coming from the field
    20 is usually accompanied by a series of foreign elements foreign to the fruit, such as soil, stones, branches or possible metallic elements. Cleaning is carried out manually and mechanically.
    b) Thick chopping, in a hammer mill, adjusted to break the pod into pieces of adequate size, without damaging as far as possible the seed or garrofín, which separates intact from the pod.
    c) Separation of pod and seed, separating the seed from the thick pieces of pod.
    d) Thin slicing, bringing the thick sheath pieces to a new hammer chopper that crushes them to the right size for proper operation
    5 extraction (approximately 0.5 centimeters in diameter), reaching a
    Engagement size such that extraction times are not too long, but the amount of fines produced is also not excessive.
    e) Aqueous extraction of the water-soluble components of the sheath, with low contact times, from 30 to 45 minutes, insufficient for the proliferation of microorganisms, avoiding unwanted fermentation and other
    abnormal biological processes.
    f) Pressing, as efficient as possible in order to extract as much
    of juice.
    g) Coarse filtering, in order to remove the significant solids load of
    15 varied sizes that drag the juice after the pressing operation, using sieves arranged sequentially, from more than 300 microns, to about 40 microns.
    h) Ultrafiltration of the juice from the previous stage (g) through membranes,
    obtaining a juice permeated by pores of 1 KDalton or less, and also of 5,
    20 8, 15, 50 and 150 KDalton or in that range, which is a totally clean product of suspended solids, with a color load much less intense than the juice of the previous stage, and more pleasant smell and taste properties .
    i) Concentration of juice from stage h to levels of 65-75 Brix
    approximately, to obtain a marketable syrup of pleasant taste and smell containing carbohydrates, micronutrients and polyphenols
    Natural refined water-soluble carob pod.
    j) Treatment with an adsorbent agent, such as activated carbon or resins
    neutral, of the ultrafiltered juice in stage h, in order to improve its organoleptic properties.
    k) Concentration of stage j juice to levels of 65-75 Brix
    approximately, to obtain a second marketable flavor syrup and
    Pleasant odor containing carbohydrates, micronutrients and polyphenols 5 natural refined water-soluble carob pod, finer than in step i).
    [3]
    3. Uses of the pleasant taste and odor syrup containing carbohydrates, micronutrients and natural refined water-soluble polyphenols of the carob pod, according to claim 1, in those applications similar to those
    10 contemplated for other sugars or sugar syrups of natural origin.
    [4 ]
    Four . Use of the carob fruit to obtain a pleasant flavor and smell syrup containing carbohydrates, micronutrients and natural refined water-soluble polyphenols of the carob pod according to
    15 procedure of claims 1 to 2.
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    同族专利:
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    ES2060544A1|1993-03-26|1994-11-16|Cia Gral Del Algarrobo De Espa|A syrup consisting of natural carob sugars and a process for its production.|
    DE19619844A1|1996-05-17|1997-11-20|Davduv Gmbh|Preparation of carob tree fruit food product used as e.g. sweetener, pudding or bread spread|
    ES2284381A1|2006-03-15|2007-11-01|Compañia General Del Algarrobo De España S.A.|Sugar extract and cyclitole obtaining method involves extraction with fluid in supercritical pressure and temperature conditions, which are modified for complete purification achieved by ion exchange chromatography|
    WO2020141235A1|2019-01-02|2020-07-09|Gregorio Martinez-Fortun, S.L|Syrup having a pleasant flavour and aroma containing natural refined polyphenols, carbohydrates and micronutrients from carob and production method|
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