JPH04100536A - W/o/w type composite emulsion and preparation thereof - Google Patents
W/o/w type composite emulsion and preparation thereofInfo
- Publication number
- JPH04100536A JPH04100536A JP2215881A JP21588190A JPH04100536A JP H04100536 A JPH04100536 A JP H04100536A JP 2215881 A JP2215881 A JP 2215881A JP 21588190 A JP21588190 A JP 21588190A JP H04100536 A JPH04100536 A JP H04100536A
- Authority
- JP
- Japan
- Prior art keywords
- porous membrane
- type composite
- emulsion
- composite emulsion
- pores
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000839 emulsion Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title description 2
- 239000012528 membrane Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000011148 porous material Substances 0.000 claims abstract description 27
- -1 ricinoleic acid ester Chemical class 0.000 claims description 22
- 239000008346 aqueous phase Substances 0.000 claims description 17
- 239000012071 phase Substances 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 229960003656 ricinoleic acid Drugs 0.000 claims description 13
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 claims description 13
- 229940066675 ricinoleate Drugs 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 6
- WBHHMMIMDMUBKC-QJWNTBNXSA-M ricinoleate Chemical compound CCCCCC[C@@H](O)C\C=C/CCCCCCCC([O-])=O WBHHMMIMDMUBKC-QJWNTBNXSA-M 0.000 claims 2
- 150000002148 esters Chemical class 0.000 abstract 2
- 239000003995 emulsifying agent Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 13
- 238000004945 emulsification Methods 0.000 description 10
- 239000005288 shirasu porous glass Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000000265 homogenisation Methods 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 241000606270 Valerianella Species 0.000 description 3
- 235000003560 Valerianella locusta Nutrition 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000005373 porous glass Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 102000011632 Caseins Human genes 0.000 description 2
- 108010076119 Caseins Proteins 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229940080237 sodium caseinate Drugs 0.000 description 2
- 238000006227 trimethylsilylation reaction Methods 0.000 description 2
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 239000008307 w/o/w-emulsion Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/4105—Methods of emulsifying
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Cosmetics (AREA)
- Colloid Chemistry (AREA)
- General Preparation And Processing Of Foods (AREA)
- Medicinal Preparation (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明ハ、Ｗ／Ｏ／Ｗ型複合エマルション及びその製造
法に関するものであり１本発明に係るＷ／Ｏ／Ｗ型複合
二マルションは、化粧品、医薬品や飲食品をはじめとす
る各種の産業分野において有用である。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a W/O/W type composite emulsion and a method for producing the same. It is useful in various industrial fields including cosmetics, pharmaceuticals, and food and drink products.
（従来の技術及び問題点）
Ｗ／Ｏ／Ｗ型複合エマルションの調製にあたり、本発明
者らは、ポリグリセリン縮合リシノレイン酸エステルを
使用することにより、生成率が高くしかも安定性にすぐ
れたエマルションを創製するのに成功し、（特開昭６０
−１６５４６号）、食品の製造技術分野において利用し
ている。(Prior art and problems) In preparing a W/O/W type composite emulsion, the present inventors created an emulsion with a high production rate and excellent stability by using polyglycerin condensed ricinoleate ester. succeeded in creating the
-16546) and is used in the food manufacturing technology field.
しかしながら、上記発明は未だ完全なものではなく、生
成する複合エマルションの粒子径の分布の幅を小さくす
るには、従来の均質化機を使用した均質化では限界があ
る。また微細なエマルションを得ようとする程せん断の
強度、時間共により多く必要となり内水の放呂の度合が
大きくなるため、大きい脂肪球程内水が入り易く、小さ
い脂肪球程内水が入りにくい傾向がある。However, the above invention is not yet perfect, and homogenization using a conventional homogenizer has a limit in reducing the width of the particle size distribution of the composite emulsion produced. In addition, the greater the shear strength and time needed to obtain a fine emulsion, the greater the degree of shearing, so the larger the fat globules, the more water will enter, and the smaller the fat globules, the more water will enter. It tends to be difficult.
（問題点を解決するための手段）
本発明はこれらの欠点を一挙に解決するためになされた
ものであって、少量の乳化剤を使用するにもかかわらず
、生成した複合エマルションの粒子径は微細且つ均一に
揃っており、そのうえ内水の大きさ及び封入量も均一に
揃っている従来未知のＷ／Ｏ／Ｗ型複合エマルションを
、簡単な操作で製造する目的でなされたものである。(Means for Solving the Problems) The present invention was made to solve these drawbacks all at once, and despite using a small amount of emulsifier, the particle size of the produced composite emulsion is fine. This was done for the purpose of producing a conventionally unknown W/O/W type composite emulsion in which the internal water is uniform and the size and amount of water enclosed are also uniform, with a simple operation.
そこで上記目的達成のために各方面から研究の結果、ポ
リグリセリン縮合リシノレイン酸エステルを使用して調
製したＷ／Ｏ組成物を細孔を有する多孔質膜を通して外
水中に分散させる。あるいはＷ／Ｏ組成物中に水を更に
分散させて転相させることで、微小で均一なＷ／Ｏ／Ｗ
型複合エマルシコンが得られる、という新知見を得、こ
の新知見を基礎として更に研究の結果、本発明は完成さ
れたのである。Therefore, in order to achieve the above object, as a result of various studies, a W/O composition prepared using polyglycerin condensed ricinoleic acid ester was dispersed in open water through a porous membrane having pores. Alternatively, by further dispersing water in the W/O composition and inverting the phase, fine and uniform W/O/W
The present invention was completed as a result of further research based on the new knowledge that a type composite emulsicone can be obtained.
すなわち本発明は、Ｗ／Ｏ／Ｗ型複合エマルションの調
製をポリグリセリン縮合リシノレイン酸エステルと細孔
を有する多孔質膜を併用して行うことを基本的技術思想
とするものである。That is, the basic technical idea of the present invention is to prepare a W/O/W type composite emulsion using a polyglycerin condensed ricinoleate ester and a porous membrane having pores.
以下１本発明を更に詳しく説明することとする。The present invention will be explained in more detail below.
本発明においては先ずはじめに、水、油脂及び乳化剤を
用いて１次乳化を行ってＷ／Ｏ型エマルションとする。In the present invention, first, primary emulsification is performed using water, oil and fat, and an emulsifier to form a W/O emulsion.
この場合、水には各種添加物、添加料等を加えて水相と
しておいてもよく、また加温しておいてもよい。油脂と
しては、油脂、脂肪酸等の油性物質であればいがなるも
のでもよいが。In this case, various additives, additives, etc. may be added to the water to form an aqueous phase, or the water may be heated. The oil may be any oily substance such as oil or fatty acid.
硬化油を用いる場合は、加温溶融して使用する。When using hydrogenated oil, heat and melt it before use.
油脂には乳化剤を溶解せしめて油相としてもよいし、ま
た水又は水相に乳化剤を分散せしめてもよいし、必要あ
れば水相及び油相の双方に乳化剤を添加してもよい。An emulsifier may be dissolved in the oil or fat to form an oil phase, or an emulsifier may be dispersed in water or an aqueous phase, or if necessary, an emulsifier may be added to both the aqueous phase and the oil phase.
本発明においては、乳化剤としてポリグリセリン縮合リ
シノレイン酸エステルを使用する６ポリグリセリン縮合
リシノレイン酸エステルとしては、テトラグリセリン縮
合リシノレイン酸エステル、ヘキサグリセリン縮合リシ
ノレイン酸エステル、デカグリセリン縮合リシノレイン
酸エステルなどがあるが、これらのいずれでもよく、ま
た混合物でもよい。In the present invention, the 6-polyglycerin condensed ricinoleate ester used as an emulsifier includes tetraglycerin condensed ricinoleate ester, hexaglycerin condensed ricinoleate ester, decaglycerin condensed ricinoleate ester, etc. , any one of these may be used, or a mixture may be used.
この乳化剤は、上記のようにＷ／Ｏ型エマルションを製
造するための１次乳化の際に使Ｉｌｆ＋するものである
が、必要あればＷ／Ｏ／Ｗ型腹合エマルションを製造す
るための２次乳化の際にも使用可能である。乳化剤は、
対油０．１〜５％、好ましくは０．７〜２．５％、更に
好ましくは１．０〜２．３％添加、混合される。対水の
場合もこれに準じて行う６本発明においては乳化剤とし
てポリグリセリン縮合リシノレイン酸エステルを使用し
なければならないが、更に他の親水性及び／又は親油性
乳化剤の併用を妨げるものではない。This emulsifier is used in the primary emulsification to produce the W/O emulsion as described above, but if necessary, it can be used in the secondary emulsification to produce the W/O/W emulsion. It can also be used during subsequent emulsification. The emulsifier is
It is added and mixed in an amount of 0.1 to 5%, preferably 0.7 to 2.5%, more preferably 1.0 to 2.3% based on oil. The same applies to the case of water.6 In the present invention, polyglycerin condensed ricinoleic acid ester must be used as an emulsifier, but this does not preclude the use of other hydrophilic and/or lipophilic emulsifiers in combination.
本発明においては、Ｗ／Ｏ型エマルションを製造するの
に２つの方法がある。第１は、油脂に水相を逐次添加混
合して、直接Ｗ２Ｏ型のエマルションとする方法であり
、第２は水相に油相を逐次添加混合して、まず０／ｗ型
のエマルションとし、これをよく攪拌して転相を起させ
て、Ｗ２Ｏ型のエマルションとする方法である。In the present invention, there are two methods for producing the W/O type emulsion. The first method is to sequentially add and mix an aqueous phase to oil and fat to directly form a W2O type emulsion, and the second method is to sequentially add and mix an oil phase to an aqueous phase to first form a 0/w type emulsion. This is a method in which the mixture is thoroughly stirred to cause phase inversion to form a W2O type emulsion.
これらの方法を実施するには、常法にしたがって乳化機
を使用して行ってもよいが、細孔を有する多孔質膜を利
用してもよい。特に、多孔質膜と乳化剤としてポリグリ
セリン縮合リシノレイン酸エステルを併用することによ
り、上述のいずれの方法によっても微細水滴を有するＷ
／Ｏ型エマルションを得ることができるが、転相による
第２の方法によれば、更に微細で均一な水滴が得られる
。To carry out these methods, an emulsifying machine may be used in accordance with a conventional method, or a porous membrane having pores may be used. In particular, by using a porous membrane and polyglycerin condensed ricinoleic acid ester as an emulsifier, W with fine water droplets can be obtained by any of the above methods.
/O type emulsion can be obtained, but according to the second method by phase inversion, even finer and more uniform water droplets can be obtained.
微細な乳化物を得るには、−度に多量混合しない方が好
ましく、また油脂と水との使用比率は、油脂：水＝３：
１〜１：３程度の割合とするのが好適であるが、上記範
囲のみレニ限定されるものではない。In order to obtain a fine emulsion, it is preferable not to mix a large amount at once, and the ratio of oil and water used is 3: oil and water.
A ratio of about 1 to 1:3 is preferable, but the ratio is not limited to the above range.
上記したように、均一な細孔を有する多孔質膜を用いて
エマルションの調製を行うと、特に粒子径の分布幅の狭
い均一なエマルションが得られる。As described above, when an emulsion is prepared using a porous membrane having uniform pores, a uniform emulsion with a particularly narrow particle size distribution can be obtained.
本発明で使用する多孔質膜としては、平均細孔径が１．
０μ閣以下であり全細孔の８０％以上が平均細孔径の０
．８〜１．２倍の間に存在するものが好適である。した
がって、多孔質ガラス、その（アミノ）シラン誘導体、
活性炭、酸性白土、カオリナイト、ベントナイト、アル
ミナ、シリカゲル、ヒドロキシルアパタイトその他の無
機ないし有機多孔体が広く使用でき、特に上記要件に適
合するものであれば更にイイ利に使用することができる
。The porous membrane used in the present invention has an average pore diameter of 1.
The average pore diameter is 0μ or less, and more than 80% of all pores have an average pore diameter of 0.
．． Those present between 8 and 1.2 times are preferred. Therefore, porous glasses, their (amino)silane derivatives,
Activated carbon, acid clay, kaolinite, bentonite, alumina, silica gel, hydroxylapatite and other inorganic or organic porous materials can be widely used, and in particular, those that meet the above requirements can be used more advantageously.
多孔質膜の好適例としては、シラス多孔質ガラス（略称
ｓｐｃ ：宮崎系工業試験＠）からなるＳＰＧ膜が挙げ
ら九る。ＳＰＧ膜は、強度、細孔径の均−性等の面で特
にすぐれているので、本発明で使用するのに好適である
。ＳＰＧ膜としては、アミノシラン化したり、オクタデ
シルシリル化や、トリメチルシリル化して疎水修飾した
ものを使用してもよい。A preferred example of the porous membrane is an SPG membrane made of Shirasu porous glass (abbreviated as SPC: Miyazaki Industry Testing). SPG membranes are particularly excellent in terms of strength, pore size uniformity, etc., and are therefore suitable for use in the present invention. The SPG film may be hydrophobically modified by aminosilanization, octadecylsilylation, or trimethylsilylation.
１次乳化終了後、２次乳化を行うのであるが、本発明に
おいては、２次乳化は上記した多孔質膜を用いて実施す
るものである。すなわち、ポリグリセリン縮合リシノレ
イン酸エステルを用いて調製したＷ／Ｏ７０組成物次乳
化）を２次乳化してＷ／Ｏ／Ｗ型複合エマルションを製
造するに際して、本発明においては、該Ｗ／Ｏ７０組成
物孔質膜を用いて外水相中に分散せしめる方法、及び該
Ｗ／Ｏ組成物１こ、多孔質膜を用いて更に水相を分散さ
せ転相させる方法のいずれか又は両方によって、目的と
するＷ／Ｏ／Ｗ型複合エマルションを得るのである。After the primary emulsification is completed, secondary emulsification is performed, and in the present invention, secondary emulsification is performed using the above-mentioned porous membrane. That is, when producing a W/O/W type composite emulsion by secondary emulsification of a W/O70 composition prepared using polyglycerin condensed ricinoleate ester, in the present invention, the W/O70 composition The objective can be achieved by either or both of a method of dispersing the W/O composition 1 into the external aqueous phase using a porous membrane, and a method of further dispersing the aqueous phase using a porous membrane and inverting the phase. A W/O/W type composite emulsion is obtained.
なお本発明において、細孔を有する多孔質膜の使用はＷ
／Ｏ組成物の外水への分散に使用することのみに制限さ
れず、油相への水相の添加、水相への油相の添加、Ｗ／
Ｏ組成物への水相の添加にも使用される。In the present invention, the use of a porous membrane having pores is W.
The use is not limited only to dispersing the /O composition in external water, but also the addition of an aqueous phase to an oil phase, the addition of an oil phase to an aqueous phase, W/
It is also used to add an aqueous phase to the O composition.
このようにして得られたＷ／Ｏ／Ｗ型複合エマルション
は、粒子の９５％以上が個数平均１重麓平均、面積平均
のいずれにおいても平均粒子径の０．５〜１．５倍の間
に存在するものであり、また、内水相の９５％以上が平
均粒子径の０．５〜１．５倍の間に存在し且つ個々の脂
肪球内に封入される水滴の意も均一であって、所期の目
的を充分に達成しつるものである。In the W/O/W type composite emulsion thus obtained, 95% or more of the particles are between 0.5 and 1.5 times the average particle diameter in both the number average and area average. In addition, 95% or more of the internal aqueous phase exists between 0.5 and 1.5 times the average particle diameter, and the water droplets enclosed within individual fat globules are also uniform. Therefore, it fully achieves its intended purpose.
従来の均質化方法では微小なエマルションを得ようとす
る程封入される内水の滴数は減少し、大きさが不均一に
なる傾向があった。In conventional homogenization methods, the smaller the emulsion is obtained, the smaller the number of encapsulated internal water droplets tends to be, and the size of the droplets tends to become non-uniform.
しかしながら本発明のように、細孔を有する多孔質膜に
よる乳化法ではＷ／Ｏ組成物を所望の粒子径に一段階で
揃えるためせん新生の内水の放出の可能性は非常に小さ
く、更に生成率の高いＷ／０／Ｗ型複合エマルションを
得ることができる。However, in the emulsification method using a porous membrane having pores as in the present invention, the possibility of releasing the internal water of the new thread is very small because the W/O composition is uniformed to the desired particle size in one step. A W/0/W type composite emulsion with a high production rate can be obtained.
個々のエマルション粒子を見ると、封入された内水の滴
数、大きさが従来法と比較してより均一となり、各々の
粒子中に含まれる薬剤量が均一となるという利点がある
。When looking at individual emulsion particles, there is an advantage that the number and size of encapsulated internal water droplets are more uniform compared to conventional methods, and the amount of drug contained in each particle is uniform.
また、生成したＷ／Ｏ／Ｗ型複合エマルションの粒子径
と比重が均一であるので、粒子径差に由来する凝集、合
一による乳化の不安定化の度合が非・常に小さくなる。Furthermore, since the particle size and specific gravity of the produced W/O/W type composite emulsion are uniform, the degree of destabilization of emulsification due to aggregation and coalescence resulting from the difference in particle size is extremely small.
そして生成するＷ／Ｏ／Ｗ型複合エマルションの粒子径
は使用する多孔質膜の細孔径によって調節できるので、
所望するＷ／Ｏ／Ｗ型複合エマルションが自由にコント
ロールしながら製造、入手できる。The particle size of the W/O/W type composite emulsion produced can be adjusted by the pore size of the porous membrane used.
A desired W/O/W type composite emulsion can be produced and obtained under free control.
以下１本発明を試験例及び実施例により更に詳しく説明
する。The present invention will be explained in more detail below using test examples and examples.
試験例１
５０℃のコーンサラダ油に乳化剤として、ポリグリセリ
ン縮合リシノレイン酸エステル、デカグリセリンデカオ
レート、ソルビタンモノオレートを対油２．０％添加し
、混合溶解した。このもの２００ｇと５０℃の水／Ｏ０
ｇを混合し高速攪拌機（バイオミキサー）で／Ｏ．００
０ｒｐｍで攪拌し、超音波処理した。Test Example 1 Polyglycerin condensed ricinoleic acid ester, decaglycerin decaolate, and sorbitan monooleate were added as emulsifiers to corn salad oil at 50° C. in an amount of 2.0% based on oil, and mixed and dissolved. 200g of this and 50℃ water/O0
g and mixed with a high-speed stirrer (bio mixer)/O. 00
The mixture was stirred at 0 rpm and sonicated.
得られたＷ／Ｏ組成物を、従来法又は多孔質膜を用いて
、ナトリウムカゼイネート３．０％添加した外水相５０
０ｇに分散させＷ／Ｏ／Ｗ型複合エマルションを得た。The obtained W/O composition was added to an external aqueous phase of 50% by adding 3.0% sodium caseinate using a conventional method or a porous membrane.
0 g to obtain a W/O/W type composite emulsion.
得られた結果を表１に示す。従来法としては、Ｗ／Ｏ組
成物添加後に羽根攪拌行った後均質化機（ホモゲナイザ
ー）を使用して均質化を行った。The results obtained are shown in Table 1. In the conventional method, after adding the W/O composition, the mixture was stirred with a blade and then homogenized using a homogenizer.
多孔質膜としてはＳＰＧ膜の細孔径０．７μｍのものを
使用した。表１かられかる通り、従来通りの均質化方法
によった場合に比較してガラス多孔質膜を使用した場合
の方が、極端に粒子径が均一に揃っていることがわかる
。また、均質化時的水の合−及び放出の程度が小さいた
め、内水の大きさ、封入量がより均一となることがわか
る。また、Ｗ／Ｏ／Ｗ型複合エマルションの調製にはポ
リグリセリン縮合リシノレイン酸エステルと多孔質ガラ
ス膜を併用することが、非常に効果的であることがわか
る。As the porous membrane, an SPG membrane with a pore diameter of 0.7 μm was used. As can be seen from Table 1, it can be seen that the particle diameter is extremely uniform when a glass porous membrane is used compared to when a conventional homogenization method is used. Furthermore, it can be seen that since the degree of water combination and release during homogenization is small, the size and amount of internal water become more uniform. Furthermore, it is found that the combined use of polyglycerin condensed ricinoleic acid ester and a porous glass membrane is very effective in preparing a W/O/W type composite emulsion.
表１
調製法および乳化剤の影響
試験例２
乳化剤としてポリグリセリン縮合リシノレイン酸エステ
ルを使用して試験例１と同様に調製したＷ／Ｏ組成物を
、細孔径の異なる多孔質ガラス膜を通してＷ／Ｏ／Ｗ型
複合エマルションを調製した。その結果を表２に示す。Table 1 Preparation method and influence of emulsifier Test example 2 A W/O composition prepared in the same manner as in Test Example 1 using polyglycerin condensed ricinoleic acid ester as an emulsifier was passed through a porous glass membrane with different pore diameters. /W type composite emulsion was prepared. The results are shown in Table 2.
表２には比較の為に。Table 2 is for comparison.
ＳＰＧ膜で調製したエマルションと同程度の平均粒子径
となるように従来通りの均質化方法で調製した結果も同
時に示した。表２かられかる通りガラス多孔質膜の細孔
径を変化させると、高い生成率は保持したまま平均粒子
径を変化させることができ、また、同じ平均粒子径をも
つ従来通りの均質化方法に比較して、粒子径の分布は非
常に小さいものとなっており、所望の大きさの粒子が自
由に調製することができることがわかる。At the same time, the results of preparing the emulsion using a conventional homogenization method so as to have the same average particle diameter as the emulsion prepared using the SPG membrane are also shown. As can be seen from Table 2, by changing the pore size of the glass porous membrane, the average particle size can be changed while maintaining a high production rate. In comparison, the particle size distribution is very small, indicating that particles of desired size can be freely prepared.
内水の大きさと封入量 以下の試験例においても同じ。Size and amount of internal water The same applies to the following test examples.
試験例３
５０℃のコーンサラダ油に乳化剤として、ポリグリセリ
ン縮合リシノレイン酸エステル２．０％を添加し、混合
、溶解した。このものに、疎水修飾（オクタデシルシリ
ル化及びトリメチルシリル化）を施したガラス多孔質膜
を通して水を分散させ、Ｗ／Ｏ組成物を得た。得られた
Ｗ／Ｏ組成物をガラス多孔質膜を用いて外水中に分散さ
せＷ／Ｏ／Ｗ型複合エマルションを得た。その結果を表
３に示す。Test Example 3 2.0% polyglycerin condensed ricinoleic acid ester was added as an emulsifier to corn salad oil at 50°C, mixed and dissolved. Water was dispersed in this material through a glass porous membrane subjected to hydrophobic modification (octadecylsilylation and trimethylsilylation) to obtain a W/O composition. The obtained W/O composition was dispersed in open water using a glass porous membrane to obtain a W/O/W type composite emulsion. The results are shown in Table 3.
表３
実施例１
５０℃のコーンサラダ油／Ｏ００ｇにポリグリセリン縮
合リシノレイン酸エステル３０ｇを混合、溶解し、得ら
れた油相６００ｇにバイオミキサー／Ｏ，０ＯＯｒｐｔ
ｎの攪拌下で５０℃の水４００ｇ添加し、超音波処理を
行って／Ｏ００ｇのＷ／Ｏ７０組成物た。Table 3 Example 1 30g of polyglycerin condensed ricinoleic acid ester was mixed and dissolved in 00g of corn salad oil/O at 50°C, and 600g of the obtained oil phase was mixed with Biomixer/O,0OOOrpt.
400 g of water at 50° C. was added under stirring at 100° C., and ultrasonication was performed to obtain a W/O70 composition of 00 g/W/O70.
得られたＷ／Ｏ組成物を平均細孔径０．５μｍのＳＰＧ
膜を通して、９８０ｇの水に２０ｇのナトリウムカゼイ
ネートを溶解するとともに５０℃に加温した外水相中に
圧入し、脂肪率３０％のＷ／Ｏ／Ｗ型複合エマルション
を得た。得られたＷ／Ｏ／Ｗ型複合エマルションは、生
成率９５．５％で平均の粒子径は２．１μｌであり、１
．０〜３．０μ麿の間に全体の９９．５％が存在してい
た。また内水の粒子径は極めて均一であり、その封入数
も、はぼ一定であった。The obtained W/O composition was made into SPG with an average pore diameter of 0.5 μm.
20 g of sodium caseinate was dissolved in 980 g of water and injected into the external aqueous phase heated to 50° C. through a membrane to obtain a W/O/W type composite emulsion with a fat percentage of 30%. The obtained W/O/W type composite emulsion had a production rate of 95.5%, an average particle size of 2.1 μl, and 1
．． 99.5% of the total amount existed between 0 and 3.0 μm. In addition, the particle size of the inner water was extremely uniform, and the number of particles enclosed was also almost constant.
（発明の効果）
本発明によりはじめて微細にして粒子径の揃ったＷ／Ｏ
／Ｗ型複合エマルションを工業的に製造することが可能
となった。しかも得られたエマルションは、その内水の
粒子径も極めて均−且つその封入数もほぼ一定であり、
各粒子中に均一に薬剤等を含有させることができるので
、きめが細かく接触感もきわめてなめらかである特性と
も相まって、医薬、化粧品、飲食品等各種の技術分野で
重用されるものである。(Effect of the invention) The present invention enables W/O to be made fine and uniform in particle size for the first time.
/W type composite emulsion can now be produced industrially. Moreover, in the obtained emulsion, the particle size of the internal water is extremely uniform, and the number of particles enclosed is almost constant,
Since it is possible to uniformly contain drugs, etc. in each particle, this, combined with its fine grain and extremely smooth touch, makes it an important material in various technical fields such as medicine, cosmetics, food and beverages, etc.
代理人 弁理士 戸 １）親 男Agent Patent Attorney 1) Parent Male
Claims (9)
ノレイン酸エステルを併用することを特徴とするＷ／Ｏ
／Ｗ型複合エマルションの製造法。(1) W/O characterized in that a porous membrane having pores and a polyglycerin condensed ricinoleic acid ester are used together.
/Production method of W-type composite emulsion.
いて調製したＷ／Ｏ組成物を細孔を有する多孔質膜を用
いて外水相中に分散させることを特徴とする請求項１に
記載のＷ／Ｏ／Ｗ型複合エマルションの製造法。(2) The W/O composition according to claim 1, wherein the W/O composition prepared using the polyglycerin condensed ricinoleic acid ester is dispersed in the external aqueous phase using a porous membrane having pores. Method for producing O/W type composite emulsion.
いて調製したＷ／Ｏ組成物に、多孔質膜を用いて更に水
相を分散させ転相させることを特徴とする請求項１に記
載のＷ／Ｏ／Ｗ型複合エマルションの製造法。(3) The W/O according to claim 1, wherein the W/O composition prepared using the polyglycerin condensed ricinoleic acid ester is further dispersed and phase-inverted using a porous membrane. /Production method of W-type composite emulsion.
縮合リシノレイン酸エステルを溶解した油相中に水相を
分散せしめたエマルション、あるいは、ポリグリセリン
縮合リシノレイン酸エステルを均一に分散させた水相を
油相に分散せしめたエマルションを、Ｗ／Ｏ組成物とし
て用いることを特徴とする請求項１〜３のいずれか１項
に記載のＷ／Ｏ／Ｗ型複合エマルションの製造法。(4) An emulsion in which an aqueous phase is dispersed in an oil phase in which polyglycerin condensed ricinoleate is dissolved using a porous membrane having pores, or water in which polyglycerin condensed ricinoleate is uniformly dispersed. The method for producing a W/O/W type composite emulsion according to any one of claims 1 to 3, characterized in that an emulsion in which the phase is dispersed in an oil phase is used as the W/O composition.
縮合リシノレイン酸エステルを溶解した油相を水相に分
散させ転相せしめたエマルション、あるいはポリグリセ
リン縮合リシノレイン酸エステルを分散させた水相に油
相を分散させ転相せしめたエマルションを、Ｗ／Ｏ組成
物として用いることを特徴とする請求項１〜３のいずれ
か１項に記載のＷ／Ｏ／Ｗ型複合エマルションの製造法
。(5) An emulsion in which an oil phase in which a polyglycerin condensed ricinoleate ester is dissolved is dispersed into an aqueous phase using a porous membrane having pores, or a water phase in which a polyglycerin condensed ricinoleate ester is dispersed. The method for producing a W/O/W type composite emulsion according to any one of claims 1 to 3, characterized in that an emulsion obtained by dispersing an oil phase and inverting the phase is used as the W/O composition.
使用することを特徴とする請求項１〜５のいずれか１項
に記載のＷ／Ｏ／Ｗ型複合エマルションの製造法。(6) The method for producing a W/O/W type composite emulsion according to any one of claims 1 to 5, characterized in that a glass porous membrane is used as the porous membrane having pores.
飾したガラス多孔質膜を使用することを特徴とする請求
項６に記載のＷ／Ｏ／Ｗ型複合エマルションの製造法。(7) The method for producing a W/O/W type composite emulsion according to claim 6, wherein a glass porous membrane whose surface is hydrophobically modified is used as the porous membrane having pores.
ノレイン酸エステルとを併用して製造してなり、粒子の
９５％以上が個数平均、重量平均、面積平均のいずれに
おいても平均粒子径の０．５倍から１．５倍の間に存在
することを特徴とするＷ／Ｏ／Ｗ型複合エマルション。(8) Manufactured using a porous membrane having pores and a polyglycerin condensed ricinoleic acid ester, in which 95% or more of the particles have an average particle diameter of 0 in any of the number average, weight average, and area average. A W/O/W type composite emulsion characterized by being present between .5 times and 1.5 times.
ノレイン酸エステルとを併用して製造してなり、内水相
の９５％以上が平均粒子径の０．５倍から１．５倍の間
に存在し、かつ個々の脂肪球内に封入される水滴の量が
均一であることを特徴とするＷ／Ｏ／Ｗ型複合エマルシ
ョン。(9) Manufactured using a combination of a porous membrane having pores and polyglycerin condensed ricinoleic acid ester, in which 95% or more of the internal aqueous phase is between 0.5 and 1.5 times the average particle diameter. A W/O/W type composite emulsion characterized in that the amount of water droplets present in the fat globules and encapsulated within each fat globule is uniform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2215881A JP2772860B2 (en) | 1990-08-17 | 1990-08-17 | W / O / W composite emulsion and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2215881A JP2772860B2 (en) | 1990-08-17 | 1990-08-17 | W / O / W composite emulsion and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04100536A true JPH04100536A (en) | 1992-04-02 |
| JP2772860B2 JP2772860B2 (en) | 1998-07-09 |
Family
ID=16679806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2215881A Expired - Fee Related JP2772860B2 (en) | 1990-08-17 | 1990-08-17 | W / O / W composite emulsion and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2772860B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002043698A1 (en) * | 2000-11-29 | 2002-06-06 | Taisho Pharmaceutical Co.,Ltd. | W/o/w composite emulsion |
| WO2002043697A1 (en) * | 2000-11-29 | 2002-06-06 | Taisho Pharmaceutical Co.,Ltd. | W/o/w composite emulsion |
| WO2014178139A1 (en) * | 2013-05-01 | 2014-11-06 | キユーピー株式会社 | Composite emulsified seasoning |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5962340A (en) * | 1982-10-01 | 1984-04-09 | Meiji Milk Prod Co Ltd | Production of w/o/w type fat and oil composition |
| JPS6016546A (en) * | 1983-07-07 | 1985-01-28 | Meiji Milk Prod Co Ltd | Whipping cream and its preparation |
| JPS6041453A (en) * | 1983-08-12 | 1985-03-05 | Meiji Milk Prod Co Ltd | Preparation of w/o/w-type composite emulsion for food |
| JPS60203139A (en) * | 1984-03-27 | 1985-10-14 | Meiji Milk Prod Co Ltd | Production of w/o/w type complex emulsion for food |
| JPH0295433A (en) * | 1988-09-29 | 1990-04-06 | Miyazaki Pref Gov | Production of emulsion |
-
1990
- 1990-08-17 JP JP2215881A patent/JP2772860B2/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5962340A (en) * | 1982-10-01 | 1984-04-09 | Meiji Milk Prod Co Ltd | Production of w/o/w type fat and oil composition |
| JPS6016546A (en) * | 1983-07-07 | 1985-01-28 | Meiji Milk Prod Co Ltd | Whipping cream and its preparation |
| JPS6041453A (en) * | 1983-08-12 | 1985-03-05 | Meiji Milk Prod Co Ltd | Preparation of w/o/w-type composite emulsion for food |
| JPS60203139A (en) * | 1984-03-27 | 1985-10-14 | Meiji Milk Prod Co Ltd | Production of w/o/w type complex emulsion for food |
| JPH0295433A (en) * | 1988-09-29 | 1990-04-06 | Miyazaki Pref Gov | Production of emulsion |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002043698A1 (en) * | 2000-11-29 | 2002-06-06 | Taisho Pharmaceutical Co.,Ltd. | W/o/w composite emulsion |
| WO2002043697A1 (en) * | 2000-11-29 | 2002-06-06 | Taisho Pharmaceutical Co.,Ltd. | W/o/w composite emulsion |
| US6984691B2 (en) | 2000-11-29 | 2006-01-10 | Taisho Pharmaceutical Co., Ltd. | W/O/W composite emulsion |
| WO2014178139A1 (en) * | 2013-05-01 | 2014-11-06 | キユーピー株式会社 | Composite emulsified seasoning |
| JPWO2014178139A1 (en) * | 2013-05-01 | 2017-02-23 | キユーピー株式会社 | Compound emulsified seasoning |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2772860B2 (en) | 1998-07-09 |
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