JP2020083851A - Method for producing aloe extract - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 229940069521 aloe extract Drugs 0.000 title claims description 30
- 235000011399 aloe vera Nutrition 0.000 claims abstract description 92
- 241001116389 Aloe Species 0.000 claims abstract description 83
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000000605 extraction Methods 0.000 claims abstract description 37
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims description 31
- 239000008187 granular material Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 abstract description 30
- 239000002994 raw material Substances 0.000 abstract description 23
- 235000002378 plant sterols Nutrition 0.000 abstract description 14
- LMYZQUNLYGJIHI-SPONXPENSA-N 4alpha-methyl-5alpha-cholest-7-en-3beta-ol Chemical class C[C@@H]1[C@@H](O)CC[C@]2(C)[C@@H](CC[C@@]3([C@@H]([C@H](C)CCCC(C)C)CC[C@H]33)C)C3=CC[C@H]21 LMYZQUNLYGJIHI-SPONXPENSA-N 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 28
- 235000002961 Aloe barbadensis Nutrition 0.000 description 9
- 244000186892 Aloe vera Species 0.000 description 9
- 238000009826 distribution Methods 0.000 description 9
- LMYZQUNLYGJIHI-UHFFFAOYSA-N Methostenol Natural products CC1C(O)CCC2(C)C(CCC3(C(C(C)CCCC(C)C)CCC33)C)C3=CCC21 LMYZQUNLYGJIHI-UHFFFAOYSA-N 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- -1 lophenol compound Chemical class 0.000 description 6
- 239000002537 cosmetic Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- IYIFZADLIMVECH-QYQNSBOUSA-N (9r,10s,13r,14r,17r)-17-[(2r,5r)-5-ethyl-6-methylheptan-2-yl]-4,10,13-trimethyl-2,3,4,5,6,9,11,12,14,15,16,17-dodecahydro-1h-cyclopenta[a]phenanthren-3-ol Chemical compound CC1C(O)CC[C@]2(C)[C@@H](CC[C@@]3([C@@H]([C@H](C)CC[C@@H](CC)C(C)C)CC[C@H]33)C)C3=CCC21 IYIFZADLIMVECH-QYQNSBOUSA-N 0.000 description 2
- AOQRDALGACAKHI-KVCRWQBISA-N (9r,10s,13r,14r,17r)-17-[(2r,5s)-5,6-dimethylheptan-2-yl]-4,10,13-trimethyl-2,3,4,5,6,9,11,12,14,15,16,17-dodecahydro-1h-cyclopenta[a]phenanthren-3-ol Chemical compound CC1C(O)CC[C@]2(C)[C@@H](CC[C@@]3([C@@H]([C@H](C)CC[C@H](C)C(C)C)CC[C@H]33)C)C3=CCC21 AOQRDALGACAKHI-KVCRWQBISA-N 0.000 description 2
- AOQRDALGACAKHI-UHFFFAOYSA-N 4-methylergost-7-en-3-ol Natural products CC1C(O)CCC2(C)C(CCC3(C(C(C)CCC(C)C(C)C)CCC33)C)C3=CCC21 AOQRDALGACAKHI-UHFFFAOYSA-N 0.000 description 2
- IYIFZADLIMVECH-UHFFFAOYSA-N 4-methylstigmast-7-en-3-ol Natural products CC1C(O)CCC2(C)C(CCC3(C(C(C)CCC(CC)C(C)C)CCC33)C)C3=CCC21 IYIFZADLIMVECH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000014104 aloe vera supplement Nutrition 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000013376 functional food Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- LVGUZGTVOIAKKC-UHFFFAOYSA-N 1,1,1,2-tetrafluoroethane Chemical compound FCC(F)(F)F LVGUZGTVOIAKKC-UHFFFAOYSA-N 0.000 description 1
- 240000007474 Aloe arborescens Species 0.000 description 1
- 235000004509 Aloe arborescens Nutrition 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 230000003178 anti-diabetic effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000007884 disintegrant Substances 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000011899 heat drying method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000014366 other mixer Nutrition 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
Description
本発明は、アロエ抽出物の製造方法に関する。より具体的には、アロエ特有の機能性成分であるシクロラノスタン化合物及びロフェノール化合物等の植物ステロールを含む抽出物の製造方法に関する。 The present invention relates to a method for producing an aloe extract. More specifically, it relates to a method for producing an extract containing a plant sterol such as a cyclolanostane compound and a lophenol compound, which are functional components peculiar to aloe.
アロエはアロエ属に属する多肉植物の総称であり、３００種類以上の品種があるとされている。中でもアロエベラ（Aloe vera）は、長年、外用や内服の方法で民間療法に利用されてきた植物である。近年、アロエの有する機能性が注目され、機能性食品、サプリメント、医薬品、化粧品などへの利用が検討されている。 Aloe is a general term for succulent plants belonging to the genus Aloe, and it is said that there are over 300 varieties. Among them, Aloe vera is a plant that has been used for folk remedies for many years by external or internal use. In recent years, the functionality of aloe has attracted attention, and its use in functional foods, supplements, pharmaceuticals, cosmetics, etc. has been studied.
アロエに含有される機能性成分として、植物ステロールが知られ、中でもシクロラノスタン化合物（９，１９−シクロラノスタン−３−オール、２４−メチレン−９，１９−シクロラノスタン−３−オール）とロフェノール化合物（４−メチルコレスト−７−エン−３−オール、４−メチルエルゴスト−７−エン−３−オール、４−メチルスチグマスト−７−エン−３−オール）は、アロエに特徴的であり、抗糖尿病作用（非特許文献１）に代表されるように種々の機能性が見出されている。 Plant sterols are known as functional components contained in aloe, and among them, cyclolanostane compounds (9,19-cyclolanostane-3-ol, 24-methylene-9,19-cyclolanostane-3-ol) And lophenol compounds (4-methylcholest-7-en-3-ol, 4-methylergost-7-en-3-ol, 4-methylstigmast-7-en-3-ol) were added to aloe. It is characteristic, and various functionalities have been found as represented by the antidiabetic effect (Non-patent Document 1).
アロエに含有されるシクロラノスタン化合物やロフェノール化合物を含む抽出物を得る方法として、特許文献１には、アロエベラの葉肉部分を凍結乾燥又は熱風乾燥し、水分を除去して粉末アロエベラ葉肉を調製し、調製した粉末アロエベラ葉肉から、超臨界抽出法によりアロエベラ抽出物を抽出するアロエベラ抽出物の製造方法が記載されている。 As a method for obtaining an extract containing a cyclolanostane compound or a rophenol compound contained in aloe, Patent Document 1 discloses that aloe vera mesophyll part is freeze-dried or hot-air dried to remove water to prepare powdered aloe vera mesophyll. Then, a method for producing an Aloe vera extract by extracting the Aloe vera extract from the prepared powdered Aloe vera mesophyll by a supercritical extraction method is described.
本発明は、アロエ葉肉を原料に用いる超臨界抽出又は亜臨界抽出において、シクロラノスタン化合物やロフェノール化合物等の植物ステロールの抽出効率を向上させる技術を提供することを課題とする。
本発明は、特に、アロエ葉肉の粉末として、平均粒子径が１００μｍ以下の微細な粉末を用いて超臨界抽出を行う場合に、シクロラノスタン化合物やロフェノール化合物等の植物ステロールの抽出効率を向上させる技術を提供することを課題とする。
It is an object of the present invention to provide a technique for improving the extraction efficiency of plant sterols such as cyclolanostane compounds and rophenol compounds in supercritical extraction or subcritical extraction using aloe mesophyll as a raw material.
The present invention particularly improves the extraction efficiency of plant sterols such as cyclolanostane compounds and rophenol compounds when performing supercritical extraction using a fine powder having an average particle size of 100 μm or less as powder of aloe mesophyll. It is an object to provide the technology that makes it possible.
また、本発明は、アロエ葉肉に含まれるシクロラノスタン化合物やロフェノール化合物等の植物ステロールの抽出のために有用な原料を提供すること、そのような原料の製造方法を提供することを課題とする。 Further, the present invention provides a useful raw material for the extraction of plant sterols such as cyclolanostane compounds and lophenol compounds contained in aloe mesophyll, and to provide a method for producing such a raw material. To do.
本発明者らは、アロエ葉肉の粉末から造粒物を調製し、この造粒物に対し超臨界抽出を行うことで、シクロラノスタン化合物やロフェノール化合物等の植物ステロールを効率よく抽出できることを見出し、以下の発明を完成させた。 The present inventors prepared a granulated product from aloe mesophyll powder, and by performing supercritical extraction on this granulated product, it is possible to efficiently extract plant sterols such as cyclolanostane compounds and lophenol compounds. Heading, the following inventions were completed.
すなわち、前記課題を解決する本発明は、アロエ葉肉の粉末の造粒物に対し、超臨界抽出法又は亜臨界抽出法を用いた抽出操作を行うことを含む、アロエ抽出物の製造方法である。
本発明のアロエ抽出物の製造方法によれば、アロエ葉肉に含まれるシクロラノスタン化合物やロフェノール化合物等の植物ステロールを効率よく抽出できる。
That is, the present invention for solving the above-mentioned problems is a method for producing an aloe extract, which comprises performing an extraction operation using a supercritical extraction method or a subcritical extraction method on a granulated product of aloe mesophyll powder. .
According to the method for producing an aloe extract of the present invention, plant sterols such as cyclolanostane compounds and lophenol compounds contained in aloe mesophyll can be efficiently extracted.
本発明の好ましい形態では、前記抽出操作は、溶媒として二酸化炭素を用いる。
二酸化炭素は、超臨界状態又は亜臨界状態とすることが比較的容易であり、化学的に不活性で毒性がない溶媒であることから、好適である。
In a preferred embodiment of the present invention, the extraction operation uses carbon dioxide as a solvent.
Carbon dioxide is preferable because it is relatively easy to bring it into a supercritical state or a subcritical state, and it is a chemically inert and nontoxic solvent.
本発明の好ましい形態では、本発明のアロエ抽出物の製造方法は、アロエ葉肉の粉末と水とを混合することにより、前記造粒物を得ることをさらに含む。
このような工程により造粒物を得ることにより、アロエ葉肉に含まれるシクロラノスタン化合物やロフェノール化合物等の植物ステロールを効率よく抽出できる。
In a preferred embodiment of the present invention, the method for producing an aloe extract of the present invention further comprises mixing the powder of aloe mesophyll and water to obtain the granulated product.
By obtaining a granulated product by such a step, plant sterols such as cyclolanostane compounds and lophenol compounds contained in aloe mesophyll can be efficiently extracted.
本発明の好ましい形態では、前記アロエ葉肉の粉末と水との混合比率は、粉末に対し、水が２０〜４０質量％である。
これにより、アロエ葉肉に含まれるシクロラノスタン化合物やロフェノール化合物等の脂溶性成分を効率よく抽出できる。
In a preferred embodiment of the present invention, the mixing ratio of the powder of the aloe mesophyll and water is 20 to 40% by mass with respect to the powder.
As a result, fat-soluble components such as cyclolanostane compounds and lophenol compounds contained in aloe mesophyll can be efficiently extracted.
本発明の好ましい形態では、前記アロエ葉肉の粉末のメディアン径は１００μｍ以下である。
後述する実施例で比較例として示すように、メディアン径が１００μｍ以下の比較的微細な粉末を抽出原料として超臨界抽出を行おうとすると、抽出が困難であることが確認されている。従って、このような原料からアロエ抽出物を得ようとする場合に、本発明が特に有用である。
In a preferred embodiment of the present invention, the median diameter of the aloe mesophyll powder is 100 μm or less.
As shown as a comparative example in Examples described later, it has been confirmed that extraction is difficult when attempting supercritical extraction using a relatively fine powder having a median diameter of 100 μm or less as an extraction raw material. Therefore, the present invention is particularly useful when an aloe extract is to be obtained from such a raw material.
本発明の好ましい形態では、前記造粒物は、固形分に対するアロエ葉肉由来の固形分の含有割合が、７０質量％以上である。
造粒物中の固形分の一定量以上をアロエ葉肉の粉末で構成することで、アロエ葉肉に含まれるシクロラノスタン化合物やロフェノール化合物等の植物ステロールを効率よく抽出できる。
In a preferred embodiment of the present invention, the granulated product has a content ratio of the solid content derived from aloe mesophyll with respect to the solid content of 70% by mass or more.
By configuring a certain amount or more of the solid content in the granulated product with the powder of aloe mesophyll, plant sterols such as cyclolanostane compounds and lophenol compounds contained in aloe mesophyll can be efficiently extracted.
本発明の好ましい形態では、前記造粒物は、粒子径２ｍｍ以上４ｍｍ未満の範囲内の粒子を２０質量％以上含む。
造粒物の粒子径分布を前記範囲内とすることで、アロエ葉肉に含まれるシクロラノスタン化合物やロフェノール化合物等の植物ステロールを効率よく抽出できる。
In a preferred embodiment of the present invention, the granulated product contains 20% by mass or more of particles having a particle diameter of 2 mm or more and less than 4 mm.
By controlling the particle size distribution of the granulated product within the above range, plant sterols such as cyclolanostane compounds and rophenol compounds contained in aloe mesophyll can be efficiently extracted.
前記課題を解決する本発明は、固形分に対するアロエ葉肉由来の固形分の含有割合が、７０質量％以上である、アロエ葉肉の粉末の造粒物（本明細書において「アロエ造粒物」ともいう。）である。
本発明のアロエ造粒物は、超臨界抽出又は亜臨界抽出の原料として好適である。
The present invention for solving the above-mentioned problems, the content ratio of the solid content derived from aloe mesophyll to the solid content is 70 mass% or more, a granulated product of aloe mesophyll powder (also referred to as “aloe granulated product” in the present specification). I say.).
The aloe granulated product of the present invention is suitable as a raw material for supercritical extraction or subcritical extraction.
本発明の好ましい形態では、前記アロエ造粒物は、粒子径２ｍｍ以上４ｍｍ未満の範囲内の粒子を２０質量％以上含む。
このようなアロエ造粒物は、超臨界抽出又は亜臨界抽出の原料として好適である。
In a preferred mode of the present invention, the aloe granule contains 20 mass% or more of particles having a particle diameter of 2 mm or more and less than 4 mm.
Such aloe granules are suitable as a raw material for supercritical extraction or subcritical extraction.
前記課題を解決する本発明は、アロエ葉肉の粉末と水とを混合することにより、アロエ葉肉の粉末の造粒物を得ることを含む、アロエ造粒物の製造方法である。
本発明のアロエ造粒物の製造方法によれば、超臨界抽出又は亜臨界抽出の原料を得ることができる。
The present invention for solving the above-mentioned problems is a method for producing an aloe granulated product, which comprises obtaining a granulated product of aloe mesophyll powder by mixing aloe mesophyll powder and water.
According to the method for producing an aloe granulated product of the present invention, a raw material for supercritical extraction or subcritical extraction can be obtained.
本発明によれば、アロエ葉肉に含まれるシクロラノスタン化合物及びロフェノール化合物等の植物ステロールを含むアロエ抽出物を効率よく製造することができる。また、本発明によれば、前記アロエ抽出物を製造するための原料を提供することができる。 According to the present invention, an aloe extract containing a plant sterol such as a cyclolanostane compound and a lophenol compound contained in aloe mesophyll can be efficiently produced. Further, according to the present invention, it is possible to provide a raw material for producing the aloe extract.
次に、本発明の好ましい実施形態について詳細に説明する。ただし、本発明は以下の好ましい実施形態に限定されず、本発明の範囲内で自由に変更することができるものである。尚、本明細書において百分率は特に断りのない限り質量による表示である。 Next, preferred embodiments of the present invention will be described in detail. However, the present invention is not limited to the following preferred embodiments and can be freely modified within the scope of the present invention. In this specification, percentages are expressed by mass unless otherwise specified.
本発明のアロエ抽出物の製造方法は、アロエ造粒物に対し、超臨界抽出法又は亜臨界抽出法を用いた抽出操作を行うことを含む。 The method for producing an aloe extract of the present invention includes subjecting an aloe granulated product to an extraction operation using a supercritical extraction method or a subcritical extraction method.
（１）アロエ造粒物
本発明の製造方法に用いられるアロエ造粒物は、アロエ葉肉の粉末粒子（一次粒子）が結着、凝集した粒子（二次粒子）である。
アロエ造粒物の固形分におけるアロエ葉肉由来の固形分の含有割合は、好ましくは７０質量％以上、より好ましくは８０質量％以上、さらに好ましくは９０質量％以上、さらに好ましくは９３質量％以上、さらに好ましくは９５質量％以上、特に好ましくは９８質量％以上であり、１００質量％であってもよい。アロエ造粒物中の固形分におけるアロエ葉肉由来の固形分の含有割合を高めることで、抽出原料（造粒物）に対する植物ステロールの回収率を高めることができる。なお、固形分含量は、水分含量以外の成分含量であり、直接加熱乾燥法により測定された水分含量から算出することができる（算出式：１００％−水分含量＝固形分含量）。
(1) Aloe granules The aloe granules used in the production method of the present invention are particles (secondary particles) in which powder particles (primary particles) of aloe mesophyll are bound and aggregated.
The content ratio of the solid content derived from aloe mesophyll in the solid content of the aloe granules is preferably 70% by mass or more, more preferably 80% by mass or more, further preferably 90% by mass or more, further preferably 93% by mass or more, The content is more preferably 95% by mass or more, particularly preferably 98% by mass or more, and may be 100% by mass. By increasing the content ratio of the solid content derived from aloe mesophyll in the solid content in the aloe granulated product, the recovery rate of the plant sterol in the extraction raw material (granulated product) can be increased. The solid content is a content other than the water content, and can be calculated from the water content measured by the direct heat drying method (calculation formula: 100%-water content=solid content).
アロエ造粒物（二次粒子）の粒度分布は以下（Ａ）〜（Ｄ）の少なくとも一の条件を満たすことが好ましい。 The particle size distribution of the aloe granules (secondary particles) preferably satisfies at least one of the following conditions (A) to (D).
（Ａ）粒子径２ｍｍ以上の範囲の粒子が、好ましくは４０質量％以上、さらに好ましくは６０質量％以上、より好ましくは７０質量％以上、特に好ましくは８０質量％以上である。 (A) Particles having a particle diameter of 2 mm or more are preferably 40 mass% or more, more preferably 60 mass% or more, more preferably 70 mass% or more, and particularly preferably 80 mass% or more.
（Ｂ）粒子径２ｍｍ以上４ｍｍ未満の範囲の粒子が、好ましくは２０質量％以上、さらに好ましくは４０質量％以上、より好ましくは５０質量％以上、特に好ましくは６０質量％以上であり、好ましくは９０質量％以下である。 (B) Particles having a particle diameter of 2 mm or more and less than 4 mm are preferably 20% by mass or more, more preferably 40% by mass or more, more preferably 50% by mass or more, particularly preferably 60% by mass or more, and preferably It is 90 mass% or less.
（Ｃ）粒子径４ｍｍ以上の範囲の粒子が、好ましくは５質量％以上、さらに好ましくは１０質量％以上、より好ましくは１５質量％以上、特に好ましくは２５質量％以上であり、好ましくは５０質量％以下、さらに好ましくは４０質量％以下である。 (C) Particles having a particle diameter of 4 mm or more are preferably 5% by mass or more, more preferably 10% by mass or more, more preferably 15% by mass or more, particularly preferably 25% by mass or more, and preferably 50% by mass. % Or less, more preferably 40% by mass or less.
（Ｄ）粒子径２ｍｍ未満の範囲の粒子が、好ましくは６０質量％以下、さらに好ましくは４０質量％以下、より好ましくは３０質量％以下、特に好ましくは２０質量％以下である。 (D) Particles having a particle diameter of less than 2 mm are preferably 60% by mass or less, more preferably 40% by mass or less, more preferably 30% by mass or less, and particularly preferably 20% by mass or less.
アロエ造粒物の嵩密度は、好ましくは０．３〜１．０ｇ／ｍｌ、さらに好ましくは０．４〜０．６ｇ／ｍｌである。 The bulk density of the aloe granule is preferably 0.3 to 1.0 g/ml, more preferably 0.4 to 0.6 g/ml.
以下、アロエ造粒物の原料であるアロエ葉肉の粉末について説明する。
アロエ葉肉の粉末は、例えば、常法によりアロエ属（Aloe）に属する植物から得られる葉肉を洗浄し、乾燥し、粉砕することにより得られる。アロエ属に属する植物としては、好ましくはアロエベラ（Aloe vera）、キダチアロエ（Aloe arborescens）が挙げられる。
Hereinafter, the powder of aloe mesophyll, which is a raw material of the aloe granule, will be described.
The powder of aloe mesophyll is obtained, for example, by washing mesophyll obtained from a plant belonging to the genus Aloe (Aloe) by a conventional method, drying and crushing. Preferable examples of plants belonging to the genus Aloe include Aloe vera and Aloe arborescens.
アロエ葉肉の粉末は、好ましくはメディアン径（ｄ（５０））が１００μｍ以下、好ましくは５０μｍ以下、さらに好ましくは２０μｍ以下である。これは、メディアン径が１００μｍ以下の微細なアロエ葉肉の粉末に対し超臨界抽出又は亜臨界抽出を行おうとすると良好な抽出結果が得られないという課題があるためである。アロエ葉肉の粉末のメディアン径の下限値は特に制限されないが、１μｍを目安とすることができる。
メディアン径の測定には、レーザー回折式粒子径分布測定装置を用いることができ、例えば島津製作所製 粒子径分布測定装置ＳＡＬＤ−２２００を用いることができる。
The powder of aloe mesophyll preferably has a median diameter (d(50)) of 100 μm or less, preferably 50 μm or less, and more preferably 20 μm or less. This is because if a fine aloe mesophyll powder having a median diameter of 100 μm or less is subjected to supercritical extraction or subcritical extraction, a good extraction result cannot be obtained. The lower limit of the median diameter of the aloe mesophyll powder is not particularly limited, but 1 μm can be used as a guide.
A laser diffraction type particle size distribution measuring device can be used for measuring the median size, and for example, a particle size distribution measuring device SALD-2200 manufactured by Shimadzu Corporation can be used.
（２）アロエ造粒物の製造方法
アロエ造粒物は、アロエ葉肉の粉末と水とを混合することにより製造することができる。混合は、医薬や食品の工業生産に用いられるＶ型、Ｗ型、ドラム型等の混合機を用いることができる。
(2) Method for producing aloe granule The aloe granule can be produced by mixing aloe mesophyll powder with water. For mixing, a V-type, W-type, drum-type, or other mixer used for industrial production of medicines and foods can be used.
混合における水の添加量は、造粒物が製造される範囲であればよいが、アロエ葉肉の粉末に対し、好ましくは２０〜４０質量％、さらに好ましくは２５〜３５質量％、より好ましくは２５〜３０質量％である。 The amount of water added in the mixing may be within the range where a granulated product is produced, but is preferably 20 to 40% by mass, more preferably 25 to 35% by mass, and more preferably 25% by mass relative to the powder of aloe mesophyll. Is about 30% by mass.
アロエ葉肉の粉末と水とは、各々所定量を一度に混合機に入れて混合操作を開始してもよいし、粉末を混合機に入れ、混合操作を行いながら水を徐々に添加して混合操作をしてもよい。
十分に混合を行うことにより、一定量の範囲の粉末が凝集し、造粒物が形成される。混合時間の目安は、混合機の容量の大きさ、粉末の量に応じて適宜決定することができる。混合を開始し、一定時間経過すると、造粒物が形成され始め、更に混合を続けると粒子形状の変化がほとんど生じなくなる。この時点で、混合を停止すればよい。
例えば、数十ｋｇ容量のＶ型混合機の場合には、通常、１０〜３０分、好ましくは１０〜２０分程度混合すればよい。
The powder of aloe mesophyll and water may be put in a mixer at a time to start the mixing operation, or the powder may be put in the mixer and mixed by gradually adding water while performing the mixing operation. You may operate.
By performing sufficient mixing, a certain amount of powder is aggregated to form a granulated product. The standard of the mixing time can be appropriately determined according to the volume of the mixer and the amount of powder. When mixing is started and a certain period of time has passed, a granulated product begins to be formed, and when mixing is further continued, the particle shape hardly changes. At this point, mixing may be stopped.
For example, in the case of a V-type mixer having a capacity of several tens of kilograms, the mixing is usually performed for 10 to 30 minutes, preferably 10 to 20 minutes.
混合時の水の温度は、常温であればよいが、５〜４０℃が好ましく、１０〜３０℃とすることがより好ましい。 The temperature of water at the time of mixing may be room temperature, but is preferably 5 to 40°C, and more preferably 10 to 30°C.
得られたアロエ造粒物は、そのままで、或いは乾燥して、後述するアロエ抽出物の抽出原料として用いることができる。 The obtained aloe granulated product can be used as it is or after being dried, as a raw material for extracting an aloe extract to be described later.
（３）抽出
本発明のアロエ抽出物の製造方法では、前述したアロエ造粒物を抽出原料として用いて、超臨界抽出又は亜臨界抽出を行う。
超臨界抽出又は亜臨界抽出に用いる溶媒としては、二酸化炭素、超臨界プロパン、超臨界エチレン、超臨界１，１，１，２−テトラフルオロエタン等が挙げられるが、アロエ抽出物を医薬、飲食品、化粧品等の原料に用いる場合には、残留溶媒の無毒性の観点から二酸化炭素が好ましい。
また、抽出温度は、好ましくは２８〜１２０℃の範囲で選択することができ、好ましくは５０〜１００℃、さらに好ましくは７０〜９０℃である。
また、抽出圧力は、好ましくは５．５〜６０ＭＰａの範囲で選択することができ、好ましくは３０〜５５ＭＰａ、さらに好ましくは４０〜５０ＭＰａである。
また、抽出時間は、好ましくは３０〜１２０分、さらに好ましくは６０〜１００分である。
また、本発明においては、シクロラノスタン化合物及びロフェノール化合物の抽出効率を改善する観点からは、エタノール等のエントレーナーを使用することも可能であるが、アントラキノン系化合物の含有量を少なくする観点からは、エントレーナーを使用しないことが好ましい。
(3) Extraction In the method for producing an aloe extract according to the present invention, supercritical extraction or subcritical extraction is performed using the above-mentioned aloe granule as an extraction raw material.
Examples of the solvent used for supercritical extraction or subcritical extraction include carbon dioxide, supercritical propane, supercritical ethylene, and supercritical 1,1,1,2-tetrafluoroethane. Aloe extract is a drug, food or drink. When used as a raw material for cosmetics and cosmetics, carbon dioxide is preferable from the viewpoint of nontoxicity of the residual solvent.
The extraction temperature can be selected preferably in the range of 28 to 120°C, preferably 50 to 100°C, more preferably 70 to 90°C.
The extraction pressure can be selected within the range of preferably 5.5 to 60 MPa, preferably 30 to 55 MPa, more preferably 40 to 50 MPa.
The extraction time is preferably 30 to 120 minutes, more preferably 60 to 100 minutes.
Further, in the present invention, from the viewpoint of improving the extraction efficiency of the cyclolanostane compound and the rophenol compound, it is possible to use an entrainer such as ethanol, but from the viewpoint of reducing the content of the anthraquinone compound. Therefore, it is preferable not to use an entrainer.
前述の方法により得られたアロエ抽出物においては、アロエの葉肉に含まれるシクロラノスタン化合物及びロフェノール化合物が濃縮されている。
アロエ抽出物におけるシクロラノスタン化合物及びロフェノール化合物の合計量の目安は、好ましくは０．５質量％以上、さらに好ましくは０．６質量％以上、特に好ましくは０．７質量％以上である。また、前記合計量の上限値の目安は、１質量％が目安となる。
In the aloe extract obtained by the above method, the cyclolanostane compound and lophenol compound contained in the aloe mesophyll are concentrated.
The guideline for the total amount of the cyclolanostane compound and the rophenol compound in the aloe extract is preferably 0.5% by mass or more, more preferably 0.6% by mass or more, and particularly preferably 0.7% by mass or more. The upper limit of the total amount is 1% by mass.
得られたアロエ抽出物は、そのままで、又はさらなる抽出や乾燥等の操作を経て、飲食品、化粧品、医薬等の有効成分として用いることができる。例えば、本発明のアロエ抽出物を含む医薬は、本発明のアロエ抽出物を製剤学的に許容される製剤担体等と組み合わせて適宜製造することが可能であり、製剤化にあたっては製剤担体として通常に汎用される賦形剤、結合剤、崩壊剤、滑沢剤、安定剤、矯味矯臭剤、希釈剤、界面活性剤、注射剤用溶剤等の添加剤を使用できる。 The obtained aloe extract can be used as it is or as an active ingredient of foods and drinks, cosmetics, pharmaceuticals, etc., after further operations such as extraction and drying. For example, a medicament containing the aloe extract of the present invention can be appropriately produced by combining the aloe extract of the present invention with a pharmaceutically acceptable pharmaceutical carrier, etc. Additives such as excipients, binders, disintegrants, lubricants, stabilizers, flavoring agents, diluents, surfactants, solvents for injections, etc. which are commonly used in the above can be used.
以下に実施例を用いて本発明をさらに詳しく説明するが、本発明はこれら実施例に限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
（１）アロエ造粒物の製造
以下の方法に従って、アロエ造粒物を製造した。
アロエベラの葉肉の粉末（メディアン径：５〜１５μｍ（規格範囲））８０ｇに対し、表１に示す割合で水分を添加し、３８×５３ｃｍのポリエチレン袋に入れて５分間撹拌し、造粒した。
なお、アロエベラの葉肉の粉末のメディアン径は、島津製作所製 粒子径分布測定装置ＳＡＬＤ−２２００を用いて測定した（以下の粉末の粒径について同じ）。
(1) Production of Aloe Granules Aloe granules were produced according to the following method.
Water was added at a ratio shown in Table 1 to 80 g of aloe vera mesophyll powder (median diameter: 5 to 15 μm (standard range)), the mixture was placed in a polyethylene bag of 38×53 cm, stirred for 5 minutes, and granulated.
The median diameter of the powder of Aloe vera mesophyll was measured using a particle size distribution analyzer SALD-2200 manufactured by Shimadzu (the same applies to the particle diameters of the following powders).
その結果、何れの場合であっても、造粒物が製造できた。
特に、実施例１〜３は、べたつきを生ずることなく造粒物を製造できた。
また、前記実施例１〜３の配合で、Ｖ型混合機を用いても同様に造粒ができることを別途確認した。
As a result, a granulated product could be produced in any case.
Particularly, in Examples 1 to 3, the granulated product could be produced without causing stickiness.
In addition, it was separately confirmed that, even if the V-type mixer was used in the formulations of Examples 1 to 3, the same granulation could be performed.
実施例１と実施例３のアロエ造粒物について、粒度分布を測定した。粒度分布は、ふるい法によって測定した。測定は３回行った。結果を表２及び図１に示す。
なお、後述するアロエベラ葉肉の粉末についても粒度分布を測定したが、何れも２ｍｍ未満が１００％であった。
The particle size distributions of the aloe granules of Example 1 and Example 3 were measured. The particle size distribution was measured by the sieving method. The measurement was performed 3 times. The results are shown in Table 2 and FIG.
The particle size distribution of the powder of aloe vera mesophyll described below was also measured, and in all cases, the particle size of less than 2 mm was 100%.
（２）超臨界抽出
上記で得られた実施例１〜３の造粒物全量を原料として、以下の条件で超臨界抽出を行った。
比較例として、造粒物の原料として用いたアロエベラ葉肉の粉末（メディアン径：５〜１５μｍ（規格範囲））に対しても同条件で超臨界抽出を行った。
(2) Supercritical extraction The supercritical extraction was performed under the following conditions using all the granulated materials of Examples 1 to 3 obtained above as raw materials.
As a comparative example, the supercritical extraction was performed under the same conditions for the aloe vera mesophyll powder (median diameter: 5 to 15 μm (standard range)) used as the raw material of the granulated product.
〔条件〕
機器：アイテック社製 超臨界抽出装置
溶媒：二酸化炭素
圧力：４５ＭＰａ
温度：８０℃
時間：８０分
エントレーナー：使用しない
〔conditions〕
Equipment: Aitec supercritical extraction device Solvent: Carbon dioxide pressure: 45 MPa
Temperature: 80°C
Time: 80 minutes Entrainer: Do not use
抽出前後で、実施例１〜３の造粒物の形状に大きな変化は見られなかった（図２）。 No significant change was observed in the shapes of the granulated products of Examples 1 to 3 before and after extraction (FIG. 2 ).
（３）測定
得られたアロエ抽出物に含まれるシクロラノスタン化合物（９，１９−シクロラノスタン−３−オール、２４−メチレン−９，１９−シクロラノスタン−３−オール）及びロフェノール化合物（４−メチルコレスト−７−エン−３−オール、４−メチルエルゴスト−７−エン−３−オール、４−メチルスチグマスト−７−エン−３−オール）を定量し、植物ステロール収量を算出した。
定量は、ＬＣ−ＭＳ／ＭＳを使用し、各標品を元に作成した検量線を用いて行った。結果を表３に示す。
(3) Measurement Cyclolanostane compound (9,19-cyclolanostane-3-ol, 24-methylene-9,19-cyclolanostane-3-ol) and rophenol compound contained in the obtained aloe extract (4-methylcholest-7-en-3-ol, 4-methylergost-7-en-3-ol, 4-methylstigmast-7-en-3-ol) was quantified and the plant sterol yield was determined. Calculated.
The quantification was performed using LC-MS/MS, using a calibration curve prepared based on each standard. The results are shown in Table 3.
表３からわかるように、比較例のアロエ葉肉の粉末を原料とした場合には、超臨界抽出により得られたアロエ抽出物が少なかった。これは、溶媒が原料に十分に浸透しなかったためであることも分かった。
一方、実施例のアロエ造粒物を原料とすることで、シクロラノスタン化合物及びロフェノール化合物を含むアロエ抽出物を製造できた。
以上の結果より、アロエ葉肉の粉末の造粒物を原料として超臨界抽出をすることで、シクロラノスタン化合物及びロフェノール化合物を含むアロエ抽出物を製造できることが分かった。また、アロエ造粒物の製造においては、アロエの粉末に対して２５〜３０質量％の水を添加することが特に好ましいことが分かった。
As can be seen from Table 3, when the powder of the aloe mesophyll of the comparative example was used as the raw material, the amount of the aloe extract obtained by supercritical extraction was small. It was also found that this was because the solvent did not sufficiently penetrate the raw material.
On the other hand, an aloe extract containing a cyclolanostane compound and a rophenol compound could be produced by using the aloe granulated product of Example as a raw material.
From the above results, it was found that an aloe extract containing a cyclolanostane compound and a rophenol compound can be produced by supercritical extraction using a granulated product of aloe mesophyll powder as a raw material. Further, it was found that it is particularly preferable to add 25 to 30% by mass of water to the aloe powder in the production of the aloe granules.
本発明によれば、シクロラノスタン化合物及びロフェノール化合物を高濃度に含む、アロエ抽出物の製造が可能となる。このようにして製造されたアロエ抽出物は、医薬品、飲食品、機能性食品、化粧品などの技術分野における原料として有用である。 According to the present invention, it is possible to produce an aloe extract containing a high concentration of a cyclolanostane compound and a lophenol compound. The aloe extract thus produced is useful as a raw material in the technical fields of medicines, foods and drinks, functional foods, cosmetics and the like.
Claims (10)
A method for producing an aloe granulated product, which comprises obtaining a granulated product of aloe mesophyll powder by mixing aloe mesophyll powder and water.
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| CN112057892A (en) * | 2020-08-24 | 2020-12-11 | 澳宝化妆品（惠州）有限公司 | Preparation method of aloe extract |
| CN114053198A (en) * | 2021-12-21 | 2022-02-18 | 海南荟研生物工程有限公司 | Aloe extract |
| WO2022045354A1 (en) * | 2020-08-31 | 2022-03-03 | 森永乳業株式会社 | Method for producing phytosterol starting material |
| WO2023054477A1 (en) * | 2021-09-28 | 2023-04-06 | 森永乳業株式会社 | Method for producing aloe extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112057892A (en) * | 2020-08-24 | 2020-12-11 | 澳宝化妆品（惠州）有限公司 | Preparation method of aloe extract |
| WO2022045354A1 (en) * | 2020-08-31 | 2022-03-03 | 森永乳業株式会社 | Method for producing phytosterol starting material |
| WO2023054477A1 (en) * | 2021-09-28 | 2023-04-06 | 森永乳業株式会社 | Method for producing aloe extract |
| CN114053198A (en) * | 2021-12-21 | 2022-02-18 | 海南荟研生物工程有限公司 | Aloe extract |
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