JP2010235832A - Method for removing oil from pericarp of citrus fruit, method for powdering the pericarp of citrus fruit, bath agent and functional food composed of the powder, and method for producing powdery combined product from the pericarp of citrus fruit - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for efficiently removing oil from pericarps of citrus fruits in order to provide powder of the pericarps of the citrus fruits, which has strong demands as a raw material to be added to functional foods, quasi-drugs and other functional materials. <P>SOLUTION: The method for efficiently removing oil from the pericarps of the citrus fruits comprises a step of extracting oil in the pericarps of the citrus fruits by using a high-pressure fluid to remove the oil from the pericarps of the citrus fruits. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a method for removing oil from citrus peel, a powdering method for pulverizing citrus peel, a bathing agent comprising a powder obtained by the method, a functional food, and a powder obtained by the method The present invention relates to a method for producing a composite product obtained by compounding.

  Citrus peels such as Ponkan, Iyokan, and Dekopon are highly needed as additive raw materials for functional foods, quasi drugs, and other functional materials. For example, the following patent documents 1 to Patent applications such as Patent Document 3 have been filed.

  Patent Document 1 relates to an oral intake stress-derived skin blood flow reduction improving composition, Patent Document 2 relates to a citrus extract composition, and Patent Document 3 relates to a cosmetic cleaning material. In order to use it as a preparation for such functional foods, quasi-drugs and the like, it is preferable to use powder. In fact, Patent Documents 1 to 3 disclose a technique for powdering citrus peel. It is disclosed.

  However, since the citrus peel contains a large amount of oil, there is a problem that it is difficult to dry if a general powdering technique such as freeze drying or sun drying is employed. Therefore, in order to solve such a problem, it is conceivable to perform pulverization after removing oil contained in the citrus peel in order to suitably perform pulverization. As such oil extraction and removal techniques from citrus peel, patent applications such as the following Patent Documents 4 to 6 have been made.

  Patent Document 4 relates to a method for producing polymethoxyflavones, wherein citrus peel oil is used to extract polymethoxyflavones using an organic acid aqueous solution as an extraction solvent. Patent Document 5 discloses essential oils from citrus fruits. TECHNICAL FIELD The present invention relates to a method for extraction and a vacuum distillation product extraction apparatus. Patent Document 6 relates to a method for treating citrus fruit including a skin, and freezes the citrus fruit including the skin using liquid nitrogen, and impacts the resulting frozen product. It is given and refined.

  However, since the techniques disclosed in Patent Documents 4 to 6 are techniques for the purpose of extracting the oil itself, they are not intended to be pulverized after the oil is extracted and removed. On the other hand, in order to suitably perform pulverization, the effect cannot be achieved unless the extraction and removal efficiency of the oil from the citrus peel is good. In this regard, the techniques disclosed in Patent Documents 4 to 6 are not necessarily recognized as being effective.

  In any case, conventionally, as in Patent Documents 1 to 3, although there is a technical document that discloses a technique for pulverizing citrus peel, actually, a large amount of oil is contained in the peel. Therefore, it is not easy to perform pulverization, and development of such a technique has been desired.

JP 2008-214223 A JP 2004-229528 A JP-A-5-339147 JP 2009-51738 A JP 2006-291007 A JP 2006-75115 A

  The present invention has been made to solve the above-described problems, and provides a powder of citrus peel that has a high need as an additive raw material for functional foods, quasi drugs, and other functional materials. Therefore, an object of the present invention is to provide a method for removing oil from citrus peel that can efficiently remove oil from citrus peel.

  The present invention has been made in order to solve such problems, and the oil content in the citrus peel is extracted by a high-pressure fluid and removed from the citrus peel, and is removed from the citrus peel. A method is provided.

  It is desirable to perform a pretreatment before extracting and removing the oil in the citrus peel. As the pretreatment, squeezing citrus peel is exemplified. Moreover, slurrying the citrus peel as another pretreatment is exemplified. Further, as another pretreatment, citrus peel is exemplified.

  As the citrus fruits, for example, those stored frozen are used. This is because the harvesting time of citrus fruits is limited, so that the timing of the powdering of the present invention is not limited.

  Furthermore, as citrus peels, for example, peels such as Ponkan, Iyokan and Dekopon are used. Further, it is desirable to use carbon dioxide as the fluid for increasing the pressure. Moreover, it is desirable to use a supercritical fluid or a subcritical fluid as the high-pressure fluid.

  Moreover, this invention provides the powdering method of the citrus peel characterized by pulverizing, after removing the oil in a citrus peel with a high pressure fluid. Furthermore, this invention provides the bath agent which consists of powder of the citrus fruit peel which removed the excess oil component by the above methods, or a functional food. Furthermore, the present invention provides a powdered composite product of citrus peel, wherein a powdered composite product is produced by adding the removed oil to the powdered citrus peel after the excess oil is removed by the method as described above. The manufacturing method of this is provided.

  As described above, the present invention is a method for extracting and removing the oil in the citrus peel with a high-pressure fluid, so that the oil in the citrus peel is suitably removed, and subsequent powdering and the like are performed. It is easy to carry out, and there is an effect that it is possible to easily obtain citrus peel powder having high needs as an additive material for functional foods, quasi drugs, and other functional materials. In addition, effective use of the extracted and removed oil can be achieved.

  In particular, when carbon dioxide is used as the fluid for increasing the pressure, for example, as in the conventional extraction technique using a solvent, which is one of the oil extraction techniques in citrus peel, no additional solvent is required. There is an effect that no extra cost is generated for the extraction.

  Furthermore, when a supercritical fluid or subcritical fluid is used as the high-pressure fluid, the extraction efficiency of the oil in the peel is improved, and the remaining ratio of the oil in the peel is reduced accordingly, making powdering easier. There is an effect that can be performed.

  Furthermore, before removing the oil in the citrus peel, if pre-treatment such as pressing of the citrus peel, slurrying of the citrus peel, chipping of the citrus peel, etc., the oil content of the subsequent high-pressure fluid is used. There is an effect that it can be removed more easily.

The schematic front view of the apparatus which performs the removal method of the oil from the citrus peel as one Embodiment. The schematic front view of the apparatus which performs the powdering method of the citrus peel of other embodiment. Chart of GC-MS analysis result of one embodiment Chart of GC-MS analysis results of other examples

  Hereinafter, embodiments of the present invention will be described. As described above, the method for removing oil from the citrus peel of the present invention extracts oil from the citrus peel using a high-pressure fluid and removes it from the citrus peel. In practice, excess oil in the citrus peel is extracted and removed by the high pressure fluid.

  From the viewpoint of easily removing the oil component, it is desirable to perform a pretreatment before removing the oil component in the citrus peel. Examples of the pretreatment include pressing the citrus peel, slurrying the citrus peel, and chipping the peel.

  Examples of the means for squeezing the citrus peel include a means for squeezing by arranging rollers on the top and bottom and passing the citrus peel between the top and bottom rollers.

  Generally, limonene is contained in bag-like grains called “oil vesicles” in the pericarp. In this case, if the clearance between the upper and lower rollers is made smaller than the diameter of the oil vesicle granules and squeezed, the grains are suitably crushed, and therefore limonene is preferably extracted and removed through the crushing port. Can do.

  Furthermore, as means for slurrying citrus peel, for example, an electric mixer for cooking is exemplified. Furthermore, as a means for chipping citrus peel, for example, an electric slicer for cooking is exemplified.

  Oil removal can also be performed as it is after wiping off the harvested citrus fruits without performing pretreatment such as pressing, slurrying, and chipping as described above.

  Citrus can be used as it is after harvesting, but since the harvest time is limited, it was stored frozen in order to remove the oil content and pulverization so as not to be restricted in time. Things can be used. When powdered, there is no particular hindrance to storing in a frozen state, and the quality of various products after powdering is not affected.

  As the types of citrus fruits, for example, Ponkan, Iyokan, Hassaku, Dekopon, Sweetspring, Sweet summer citrus, Satsuma mandarin, Sudachi, Persimmon, Kavos, Daidai, and other citrus fruits can be used. Furthermore, the squeezed lees remaining after manufacturing these citrus juice-containing beverages are preferably used from the viewpoint of effective use of waste. That is, the “citrus peel” in the present invention includes a squeezed rice cake remaining after manufacturing such a beverage containing citrus juice.

  As the fluid for increasing the pressure, for example, carbon dioxide, nitrous oxide, trifluoromethane, nitrogen or the like can be used. In particular, it is particularly preferable to use carbon dioxide from the viewpoint of safety in work, possibility of industrialization, and cost reduction in carrying out oil removal.

  Further, as the high-pressure fluid, it is desirable to use a supercritical fluid or a subcritical fluid from the viewpoint of increasing the oil removal efficiency. Carbon dioxide has a critical temperature of 31.1 ° C. and a critical pressure of 7.38 MPa, nitrous oxide has a critical temperature of 36.4 ° C. and a critical pressure of 7.24 MPa, and trifluoromethane has a critical temperature of 25.9 ° C. The critical pressure is 4.84 MPa, nitrogen has a critical temperature of −147 ° C. and a critical pressure of 3.39 MPa.

  In addition to the high-pressure fluid, an entrainer (auxiliary solvent) can also be added. By adding such an entrainer, the extraction efficiency can be further increased. The type of entrainer is not particularly limited.

  Furthermore, the method for pulverizing citrus peel according to the present invention is to pulverize the oil in the citrus peel after removing it with a high-pressure fluid. Moreover, the bath agent of this invention or a functional food consists of powder of the citrus peel from which the oil component was removed by the above methods.

  Furthermore, the method for producing a powdered composite product of citrus peel according to the present invention is a powder composite product obtained by adding the removed oil to the citrus peel powder from which oil has been removed by the above-described method. Is to be manufactured.

(Embodiment 1)
Next, a more specific embodiment of the method for removing oil from the citrus peel will be described with reference to FIG.

  First, the outline of the structure of the apparatus which performs the powdering method as one Embodiment is demonstrated according to FIG. As shown in FIG. 1, the apparatus for performing the powdering method of the present embodiment includes a cylinder 1, a high-pressure vessel 2, an oil recovery vessel 3, an auxiliary solvent vessel 4, two high-pressure pumps 5 and 6, A check valve 7, a back pressure valve 8, and a stop valve 15 are provided.

  The cylinder 1 is a cylinder filled with carbon dioxide as a fluid component used as a high-pressure fluid, and carbon dioxide is supplied from the cylinder 1 into the system.

  The high-pressure vessel 2 is a vessel for containing the citrus peel that is the object to be treated and removing oil, and the high-pressure fluid is brought into contact with the citrus peel inside the high-pressure vessel 2 and the crushed product of the peel. The oil is extracted and removed from. The high-pressure vessel 2 is accommodated in a thermostatic chamber 9 in order to keep the fluid components in a high-pressure fluid state.

  The oil component collection container 3 is a container for storing the oil component by separating the oil component and the component of the high pressure fluid after supplying the oil component extracted and removed by the high pressure vessel 2 and the high pressure fluid.

  The auxiliary solvent container 4 is a container for containing an auxiliary solvent for extracting and removing oil. The auxiliary solvent is supplied to the high-pressure vessel 2 by the high-pressure pump 6. As shown in FIG. 1, the auxiliary solvent is combined with the high-pressure fluid component before the high-pressure vessel 2, and the mixed fluid of the high-pressure fluid and the auxiliary solvent is supplied to the high-pressure vessel 2. Will be supplied. However, it may be supplied to the high pressure vessel 2 separately from the high pressure fluid. In either case, the mixed fluid of the high-pressure fluid and the auxiliary solvent contacts the citrus peel inside the high-pressure vessel 2 to extract and remove the oil.

  The high pressure pump 5 is for supplying the fluid component of the cylinder 1 to the high pressure vessel 2, and the pressure of the high pressure pump 5 is measured by a pressure gauge 10. The high-pressure vessel 2 is further provided with a stirrer 11 for stirring the inside. A thermometer 12 that can measure the temperature inside the high-pressure vessel 2 is also provided.

  The check valve 7 is a valve that prevents the fluid supplied to the high-pressure vessel 2 from flowing backward, and the stop valve 15 opens the flow path toward the oil recovery container 3 until the system reaches a predetermined pressure. It is a valve for closing.

  The back pressure valve 8 is for keeping the pressure in the apparatus piping on the upstream side of the back pressure valve 8 constant. Further, by opening the stop valve 15, the system and the back pressure valve 8 are brought into communication. Further, when the high-pressure pump 5 is in a flow state, when the fluid exceeding the set pressure of the back pressure valve 8 is introduced into the system, the excess fluid is discharged out of the system via the back pressure valve 8. The Rukoto.

  Next, a more specific embodiment of the method for removing oil from citrus peel using the apparatus as described above will be described.

  First, a citrus peel 13 as a processing object is accommodated in the high-pressure vessel 2. The citrus peel 13 is previously crushed by pressing. In this embodiment, Ponkan is used as citrus fruits. Next, the thermostat 9 containing the high-pressure vessel 2 is set to a predetermined temperature, the back pressure valve 8 is set to a predetermined release pressure, and then carbon dioxide is supplied from the cylinder 1 to the high-pressure vessel 2. Supply of carbon dioxide to the high-pressure vessel 2 is continuously performed by the high-pressure pump 5.

  More specifically, the pressure increased by the high-pressure pump 5 and supplied to the high-pressure vessel 2 side through the flow path becomes equal to or higher than the critical pressure, and is maintained at the pressure set by the back pressure valve 8. Yes. In order to keep the inside of the system at the set pressure, the check valve 7 prevents the fluid supplied to the high pressure vessel 2 from flowing backward to the upstream side.

  A fluid whose pressure has been raised above the critical pressure and heated above the critical temperature, that is, a supercritical fluid, is supplied to the high-pressure vessel 2. Then, the supercritical fluid supplied to the high-pressure vessel 2 extracts oil from the citrus peel ground material previously stored in the high-pressure vessel 2. In this embodiment, since Ponkan is used as citrus fruits, limonene is mainly extracted as the oil component.

  The temperature and pressure may be any conditions as long as the fluid to be used becomes a supercritical fluid, that is, a condition not lower than the critical pressure and not lower than the critical temperature. Carbon dioxide used in the present embodiment becomes a supercritical fluid under conditions of a temperature of 31.1 ° C. (critical temperature) and a pressure of 7.38 MPa (critical pressure) or higher, and the temperature setting of the thermostat as described above. The supercritical state can be maintained by setting the pressure in the back pressure valve 8. In this embodiment, the temperature is set to 40 ° C. and the pressure is set to 20 MPa.

  Then, after the temperature and pressure in the high-pressure vessel 2 reach a predetermined value (40 ° C., 20 MPa), the high-pressure pump 5 is temporarily stopped, and carbon dioxide is supplied into the system for a predetermined time (2 hours in this embodiment). To hold. At this time, the flow path to the oil recovery container 3 is closed by the stop valve 15, and carbon dioxide is not supplied to the oil recovery container 3. That is, the system is maintained at a predetermined temperature and pressure, and carbon dioxide that has become a supercritical fluid uniformly penetrates into the citrus peel fibers and cells, and the oily limonene is extracted from there. To prepare for the preparation. Furthermore, dissolution of limonene has already progressed in the permeated supercritical carbon dioxide.

  After maintaining the inside of the system for 2 hours at a temperature of 40 ° C. and a pressure of 20 MPa in this way, the flow path to the oil recovery container 3 side is opened by opening the stop valve 15, and the operation of the high-pressure pump 5 is resumed. Carbon dioxide is also circulated from the high-pressure vessel 2 to the oil recovery vessel 3 side. Then, carbon dioxide is circulated for a certain time (for example, 5 hours) in a state where the flow path to the oil recovery container 3 side is opened.

  In a state where the flow path to the oil recovery container 3 side is opened, fresh carbon dioxide is brought into contact with the citrus peel for 5 hours at a temperature of 40 ° C. and a pressure of 20 MPa, so that limonene is dissolved. It replaces critical carbon dioxide with fresh carbon dioxide. Furthermore, limonene is newly dissolved in the fresh carbon dioxide that has penetrated into the citrus peel. This cycle is then repeated for 5 hours. As a result, limonene is extracted from the citrus peel through carbon dioxide, discharged to the outside of the high-pressure vessel 2 and supplied to the oil recovery vessel 3.

  Furthermore, when it carries out on the conditions which add an auxiliary | assistant solvent, an auxiliary | assistant solvent is supplied to the high voltage | pressure container 2 via the high voltage | pressure pump 6 from the auxiliary | assistant solvent container 4 in the state which is distribute | circulating the carbon dioxide. In this embodiment, ethanol is used as the auxiliary solvent. At this time, the fluid supplied to the high-pressure vessel 2 is a mixed fluid of carbon dioxide and ethanol. Since ethanol has the effect of dissolving oily substances well, mixing with carbon dioxide, which is inherently fat-soluble, synergistically improves oil solubility. Then, a mixture of three components of supercritical carbon dioxide, ethanol, and oil (such as limonene) is supplied to the oil recovery container 3 as an extract.

  The oil collection container 3 is in communication with the atmosphere, and the pressure inside the oil collection container 3 is reduced, so that carbon dioxide becomes gas, is separated from ethanol, is discharged from the oil separation container 3, and is further out of the system. To be discharged. Then, oil (limonene or the like) is precipitated and collected in the oil collection container 3.

  As described above, in the present embodiment, the citrus peel is housed in the high-pressure vessel 2, supercritical carbon dioxide is supplied to the high-pressure vessel 2, and limonene or the like is extracted from the citrus peel by the extraction power of the supercritical carbon dioxide. Therefore, the extraction and removal rates of limonene and other oils were very good. Furthermore, the extraction rate and the removal rate were further improved by using ethanol as an auxiliary solvent for supercritical carbon dioxide.

(Embodiment 2)
This embodiment is another embodiment of a method for removing oil from citrus peel. In this embodiment, as shown in FIG. 2, the line is connected so that the oil extracted and removed in the high-pressure vessel 2 is drawn out from the bottom side of the high-pressure vessel 2 and supplied to the oil collection vessel 3. This is different from the first embodiment in which the line is connected so that the oil extracted and removed from the upper side of the high-pressure vessel 2 is drawn out and supplied to the oil collection vessel 3.

  In the present embodiment, the stirrer 11 is provided with the cocoon-like body 14, and the citrus peel 13 is accommodated in the cocoon-like body 14. As such a bowl-like body 14, there can be used a filter cloth, a mesh, a lattice, and other breathable ones so that the contained citrus peel 13 does not fall. Such a bowl-like body 14 is provided, for example, by being suspended from the stirrer 11.

  In the present embodiment, since the oil component 16 extracted and removed in the high-pressure vessel 2 is configured to be extracted from the bottom side of the high-pressure vessel 2, the oil component 16 extracted and removed is phase-separated from the supercritical fluid. Even in this case, the separated product falls to the bottom of the high-pressure vessel 2 through the cage 14. Then, the removed oil component is suitably supplied to the oil component recovery container 3 through a line on the bottom side of the high-pressure container 2. As a result, carelessly attaching the removed oil to the peel 13 is reduced.

  The point that the apparatus is configured to include the cylinder 1, the high pressure container 2, the oil recovery container 3, the auxiliary solvent container 4, the two high pressure pumps 5 and 6, the check valve 7, the back pressure valve 8, etc. Since it is the same as Form 1, the description thereof is omitted.

  Further, the action of extracting and removing oil from the citrus peel 13 contained in the high-pressure vessel 2 by the supercritical fluid is also the same as that in the first embodiment, and thus the description thereof is omitted.

(Other embodiments)
In the above embodiment, carbon dioxide (critical temperature: 31.1 ° C., critical pressure: 7.38 MPa) is used as the supercritical fluid, but in addition to this, nitrous oxide (critical temperature: 36.4 ° C., Critical pressure: 7.24 MPa), trifluoromethane (critical temperature: 25.9 ° C., critical pressure: 4.84 MPa), or the like can be used.

  In this embodiment, supercritical carbon dioxide is used as the high-pressure fluid. However, the operation conditions are less than the critical temperature and above the critical pressure, above the critical temperature and less than the critical pressure, and both the critical temperature and the critical pressure are slightly higher. It is possible to use so-called subcritical carbon dioxide, which is under a condition lower than that. Furthermore, it is possible to use a high-pressure fluid other than the supercritical fluid and the subcritical fluid.

  In the above embodiment, ethanol is used as the auxiliary solvent. However, the type of the auxiliary solvent is not limited to this. For example, lower alcohols such as methanol and propanol, hydrocarbons such as normal hexane and cyclohexane, acetone, It is also possible to use ethyl acetate or the like. In short, it is preferable to select appropriately from the viewpoint of handling substances applied in relation to foods or pharmaceuticals, and from the viewpoint of maintaining quality without deteriorating natural substances.

  Furthermore, in the above embodiment, the auxiliary solvent container 4 is provided separately from the high pressure container 2. However, without providing the auxiliary solvent container 4, for example, the auxiliary solvent is accommodated in the high pressure container 2 and the supercritical fluid is stored. May be used together.

  Furthermore, regarding the apparatus used in the above embodiment, the material of the high-pressure vessel 2 and the oil recovery vessel 3, the material of the piping, the type of equipment, and other line filters, drain valves, bypass piping, safety valves, gantry, etc. not shown General accessory parts can be selected and used as appropriate.

  Examples of the present invention will be described below.

Example 1
In this example, limonene, which is an oil component, was extracted and removed by supercritical carbon dioxide from the decapon peel as an example of citrus peel. For the extraction and removal processing, the apparatus having the configuration shown in FIG. 1 was used.

  In this example, as a sample of citrus peel, the juice squeezed cocoon of the whole decapon fruit stored at −40 ° C. in a freezer was thawed and used as it was. The squeezed trough 206 g (oil content 0.38 wt%, oil content 0.78 g) was charged into a 300 ml internal volume high pressure vessel, set at a temperature of 40 ° C. and a pressure of 20 MPa, and held for 2 hours. Thereafter, the flow rate of the high-pressure pump was circulated at 7 ml / min (liquid carbon dioxide base) for 5 hours. As a result, 0.13 g of oil could be removed. The oil removal rate at this time was 17% by weight.

  Further, as shown in FIG. 3, as a result of GC-MS analysis of the recovered oil, a limonene peak was detected at a position where the retention time was 6.8 min (min). From this, it was found that limonene was contained in the recovered oil. In FIG. 3, relatively high peaks were detected at positions other than the position where the retention time was 6.8 min, and it was found that a large amount of oil other than limonene was contained. As the GC-MS apparatus, a GCMS-QP2010 type apparatus manufactured by SHIMADZU was used. As the capillary column, CP-Sil24CB: lowbleed type (inner diameter 0.25 μm, length 30 m, media diameter 0.25 μm) was used. The column temperature was set to 50 ° C. when the sample was charged, held at that temperature for 1 minute, and then heated to 250 ° C. at a heating rate of 8 ° C./min. The sample was processed under the condition of 0.5 μl.

  In addition, the oil content was determined by mixing 100 ml of normal hexane with 10 g of dried fruit skin by a general hexane extraction method and performing osmotic extraction for 6 hours.

(Example 2)
Also in this example, the squeezed squeezed squeezed cocoon of the whole decapon fruit that had been stored in a freezer at −40 ° C. as citrus peel was used. Instead of using the thawed product as it was, a slurry of the thawed product was used. In the extraction and removal processes, the apparatus shown in FIG.

  Slurry was performed using a SB-990 type desktop super blender at 15000 rpm for 5 minutes. 204 g of the slurry (oil content: 0.27% by weight, oil content: 0.55 g) was charged into a high-pressure vessel with an internal volume of 300 ml, set at a temperature of 40 ° C. and a pressure of 20 MPa, and held for 2 hours. Thereafter, the flow rate of the high-pressure pump was circulated at 7 ml / min (liquid carbon dioxide base) for 5 hours. As a result, 0.11 g of oil could be removed. The oil removal rate at this time was 20% by weight.

  The oil content was determined in the same manner as in Example 1.

Example 3
Also in this example, the squeezed fruit juice squeezed from the whole decapon fruit preserved at −40 ° C. in a freezer as citrus peel was used. The thawing product of persimmon was not simply made into a slurry, but after removing the excess fruit contained in the thawing product, the thawing product of only the skin was made into a slurry. For the extraction and removal processes, the apparatus shown in FIG.

  Slurry was performed under the same conditions as in Example 2. 207 g of the slurry (oil content 0.19% by weight, oil content 0.39 g) was charged into a high-pressure vessel with an internal volume of 300 ml, set at a temperature of 40 ° C. and a pressure of 20 MPa, and held for 2 hours. Thereafter, the flow rate of the high-pressure pump was circulated at 7 ml / min (liquid carbon dioxide base) for 5 hours. As a result, 0.11 g of oil could be removed. The oil removal rate at this time was 28% by weight.

  The oil content was determined in the same manner as in Examples 1 and 2.

  According to the results of Examples 1 to 3 above, the raw juice squeezed from the whole decapon fruit that had been stored at −40 ° C. in a freezer was used as a raw material. Oil, the oil removal rate is 17% by weight, 20% by weight, and 28% by weight, respectively. The oil removal rate was the best when using a slurry of only the peel after removing excess fruit from the fruit juice pomace, and then the oil removal rate of the slurry of the juice pomace was good . From this, it was found that the oil content removal rate was improved by slurrying the fruit juice squeezed rather than being used as it was, and the oil content removal rate was further improved by slurrying after removing excess fruit.

Example 4
In this example, limonene, which is an oil component, was extracted and removed with supercritical carbon dioxide from Iyokan peel as an example of citrus peel. For the extraction and removal processing, the apparatus having the configuration shown in FIG. 1 was used.

  In this example, as a sample of citrus peel, a slurry obtained after removing excess fruit from a product obtained by thawing the juice squeezed from the whole Iyokan fruit preserved at −40 ° C. in a freezer was used. Slurry was performed under the same conditions as in Examples 2 and 3 above. 208 g of the slurry (oil content 0.11% by weight, oil content 0.23 g) was charged into a 300 ml internal pressure vessel, set at a temperature of 40 ° C. and a pressure of 20 MPa, and held for 2 hours. Thereafter, the flow rate of the high-pressure pump was circulated at 7 ml / min (liquid carbon dioxide base) for 5 hours. As a result, 0.07 g of oil could be removed. The oil removal rate at this time was 31% by weight.

  Further, as shown in FIG. 4, as a result of GC-MS analysis of the collected oil, a limonene peak was detected at a position where the retention time was 6.8 min (min). From this, it was found that limonene was contained in the recovered oil. In FIG. 4, almost no high peak was detected at positions other than the position where the retention time was 6.8 min. Therefore, it was found that a large amount of limonene was contained in the recovered oil. The same GC-MS apparatus and capillary column as in Example 1 were used, and the treatment was performed under the same conditions as in Example 1.

  The oil content was determined in the same manner as in Examples 1 to 3.

(Example 5)
In this example, as a sample of citrus peel, as in Example 4, after removing excess fruit from a product obtained by thawing the juice squeezed from the whole Iyokan fruit that had been stored in a freezer at minus 40 ° C., the slurry was removed. What was made into was used. While the apparatus shown in FIG. 1 was used in Examples 1 to 4, the apparatus shown in FIG. 2 was used in this example.

  Slurry was performed under the same conditions as in Examples 2 to 4. 72 g of the slurry (oil content 0.11% by weight, oil content 0.080 g) was charged into a high-pressure vessel having an internal volume of 300 ml, set at a temperature of 40 ° C. and a pressure of 20 MPa, and held for 2 hours. Thereafter, the flow rate of the high-pressure pump was circulated at 7 ml / min (liquid carbon dioxide base) for 5 hours. As a result, 0.060 g of oil could be removed. The oil removal rate at this time was 76% by weight.

  As described above, in Examples 4 and 5, the citrus peel was obtained by slurrying only the peel after removing the excess fruit from the fruit juice pomace that had the highest oil removal rate in the decopon of Examples 1 to 3. Used as a sample. As a result, when Iyokan of Examples 4 and 5 was used, an oil content removal rate higher than the highest oil content removal rate in Dekopon was shown. From the results of using the same kind of citrus peel sample, it was found that the oil removal rate with Iyokan using supercritical carbon dioxide was higher than that with Decopon. Furthermore, when the results of the apparatus shown in FIGS. 1 and 2 were compared, they were 31% by weight and 76% by weight, respectively. As an apparatus, it turned out that the effect at the time of using the apparatus of FIG. 2 is high.

DESCRIPTION OF SYMBOLS 1 Cylinder 2 High pressure container 3 Oil content collection container 4 Auxiliary solvent container 5 High pressure pump 6 High pressure pump 7 Check valve 8 Back pressure valve 13 Citrus peel

Claims (12)

  A method for removing oil from a citrus peel, wherein the oil in the citrus peel is extracted with a high-pressure fluid and removed from the citrus peel.   The method for removing oil from citrus peel according to claim 1, wherein the citrus peel is squeezed before extracting and removing the oil in the citrus peel.   The method for removing oil from citrus peel according to claim 1, wherein the citrus peel is slurried before the oil in the citrus peel is removed.   The method for removing oil from citrus peel according to claim 1, wherein the citrus peel is chipped before removing the oil in the citrus peel.   The method for removing oil from citrus peel according to any one of claims 1 to 4, wherein the citrus peel is stored frozen as citrus peel.   The method for removing oil from citrus peel according to any one of claims 1 to 5, wherein the citrus peel is Ponkan, Iyokan or Dekopon peel.   The method for removing oil from citrus peel according to any one of claims 1 to 6, wherein the fluid in a high pressure state is carbon dioxide.   The method for removing oil from citrus peel according to any one of claims 1 to 7, wherein the high-pressure fluid is a supercritical fluid or a subcritical fluid.   A method for pulverizing citrus peel, wherein oil in citrus peel is removed by high-pressure fluid and then pulverized.   The bath agent which consists of powder of the citrus peel pulverized by the powdering method of Claim 9.   A functional food comprising a powder of citrus peel peeled by the powdering method according to claim 9.   The manufacturing method of the powder compounded product of citrus peel which adds the removed oil to the powder of the citrus fruit powder pulverized by the powdering method of Claim 9, and manufactures a powder compounded product.

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