JP6154288B2 - Capsule filling composition - Google Patents
Capsule filling composition Download PDFInfo
- Publication number
- JP6154288B2 JP6154288B2 JP2013224495A JP2013224495A JP6154288B2 JP 6154288 B2 JP6154288 B2 JP 6154288B2 JP 2013224495 A JP2013224495 A JP 2013224495A JP 2013224495 A JP2013224495 A JP 2013224495A JP 6154288 B2 JP6154288 B2 JP 6154288B2
- Authority
- JP
- Japan
- Prior art keywords
- rice bran
- mass
- extract
- powder
- bran extract
- 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.)
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- 239000002775 capsule Substances 0.000 title claims description 14
- 238000011049 filling Methods 0.000 title claims description 8
- 235000007164 Oryza sativa Nutrition 0.000 claims description 50
- 235000009566 rice Nutrition 0.000 claims description 50
- 239000000284 extract Substances 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 20
- 229930182558 Sterol Natural products 0.000 claims description 15
- 235000003702 sterols Nutrition 0.000 claims description 15
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 14
- -1 sterol glycoside Chemical class 0.000 claims description 12
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- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
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Landscapes
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Description
本発明は、粉末成分を安定に分散するカプセル充填のための米糠抽出物含有組成物に関する。 The present invention relates to a rice bran extract-containing composition for capsule filling in which powder components are stably dispersed.
米糠は玄米を精白する際に出る果皮、種皮、胚芽などの部分のことである。米糠には種々の有用な成分が含有されている。代表的な成分として、フィチン酸、イノシトール、フェルラ酸、γ−オリザノール、食物繊維、蛋白質、ビタミンB1、ビタミンB6、ビタミンE、ミネラルなどを例示することができる。これらの成分を利用した米糠の抽出物配合食品や飲料が提案されている。
一方、油性溶剤に植物由来のワックス類を配合してなる基剤に、粉末成分又は水溶性成分を均一に分散してなる軟カプセル剤充填用組成物が知られている(特許文献1:特開2002−161029号公報)。
Rice bran is the part of the skin, seed coat, germ, etc. that appears when white rice is refined. Rice bran contains various useful ingredients. Representative components include phytic acid, inositol, ferulic acid, γ-oryzanol, dietary fiber, protein, vitamin B1, vitamin B6, vitamin E, mineral, and the like. Rice bran extract-containing foods and beverages using these ingredients have been proposed.
On the other hand, a composition for filling soft capsules in which a powder component or a water-soluble component is uniformly dispersed in a base obtained by blending a plant-derived wax with an oily solvent is known (Patent Document 1: Special). No. 2002-161029).
粉末成分を混合したとき、粉末成分を安定に分散させている米糠抽出物を提供することを本発明の課題とする。 It is an object of the present invention to provide a rice bran extract in which a powder component is stably dispersed when the powder component is mixed.
本発明の主な構成は、次のとおりである。
(1)アシル化ステロール配糖体を2.7〜4.1質量%、γ−オリザノールを1.4〜2.1質量%、ステアロ・オレオ・レシチン換算で、リン脂質を18〜28質量%含有し、加水分解したときに、加水分解前の質量に対して20〜30質量%のリノール酸、24〜37質量%のオレイン酸、11〜17質量%のパルミチン酸、1.7〜2.6質量%の植物ステロールを含有する米糠抽出物と
ワックス類と
粉体を
含有することを特徴とするカプセル充填用の組成物。
(2)ワックス類がミツロウである(1)に記載の組成物。
(3)粉体がβクリプトキサンチンである(1)に記載の組成物。
(4)(1)〜(3)のいずれかに記載の組成物を内包するカプセル製剤。
The main configuration of the present invention is as follows.
(1) 2.7 to 4.1% by mass of acylated sterol glycoside, 1.4 to 2.1% by mass of γ-oryzanol, and 18 to 28% by mass of phospholipid in terms of stearo, oleo and lecithin When contained and hydrolyzed, 20-30% by mass of linoleic acid, 24-37% by mass of oleic acid, 11-17% by mass of palmitic acid, 1.7-2. A capsule filling composition comprising a rice bran extract containing 6% by mass of a plant sterol, a wax and a powder.
(2) The composition according to (1), wherein the wax is beeswax.
(3) The composition according to (1), wherein the powder is β cryptoxanthin.
(4) A capsule preparation containing the composition according to any one of (1) to (3).
米糠抽出物中に配合した粉体の均一な混合状態が維持された米糠抽出物を含む組成物が提供される。この組成物は、カプセル充填適性に優れている。 There is provided a composition comprising a rice bran extract in which a uniform mixing state of the powder blended in the rice bran extract is maintained. This composition is excellent in capsule filling suitability.
本発明の組成物に含有される米糠抽出物にはアシル化ステロール配糖体が含まれている。天然物から得られるアシル化ステロール配糖体は、通常混合物である。アシル化ステロール配糖体の構成糖は主にグルコースである。
また構成ステロールはβ−シトステロール、スチグマステロール、カンペステロール等である。アシル化は主にグルコースの6位が、脂肪酸によってアシル化されており、構成脂肪酸は主にリノール酸、オレイン酸、パルミチン酸であることが明らかになっている(帯大研報,10,(1977)507〜514)。
The rice bran extract contained in the composition of the present invention contains an acylated sterol glycoside. Acylated sterol glycosides obtained from natural products are usually mixtures. The constituent sugar of the acylated sterol glycoside is mainly glucose.
The constituent sterols are β-sitosterol, stigmasterol, campesterol and the like. As for acylation, the 6-position of glucose is acylated mainly by fatty acids, and the constituent fatty acids are mainly linoleic acid, oleic acid and palmitic acid (Obihiro Lab., 10, ( 1977) 507-514).
本発明に用いられる米糠抽出物は、アシル化ステロール配糖体を2.7〜4.1質量%含有する。 The rice bran extract used in the present invention contains 2.7 to 4.1% by mass of acylated sterol glycoside.
本発明に用いられる米糠抽出物中のアシル化ステロール配糖体の含有量の測定は以下の方法により行うことができる。
(1)米糠抽出物を適量秤取し、クロロホルム/メタノール混液(クロロホルム:メタノール=2:1)を加え、メスフラスコにてメスアップする。
(2)(1)で得られた溶液は成分濃度に応じて適宜希釈し、分析用試料溶液とする。
(3)標品はEsterified Steryl Glucoside(フナコシ)とし、高速液体クロマトグラフ法によりアシル化ステロール配糖体の濃度を算出する。
(4)高速液体クロマトグラフ法による分析条件
分析装置:HPLC
移動相A:メタノール:水 = 95:5(v/v)
移動相B:クロロホルム = 100(v/v)
ポンプ:Model 582
solvent delivery system
分析カラム:LiChrospher Si60(5μm)
HPLC−Cartridge(MERCK)
検出器:荷電化粒子検出器(コロナ ダイオネクス社)
Injection Volume:20μL
カラムオーブン:40℃(FLO社 model 502)
分析時間:40min
脱泡装置:uniflows Degasys Ultimate
DV3003
流速:1mL/min
グラジェント条件
以下に示すとおり
0−15分
移動相A:1% → 25%、移動相B: 99% → 75%
15−20分
移動相A:25% → 90%、移動相B: 75% → 10%
20−25分
移動相A:90%、 移動相B: 10%
25−30分
移動相A:90% → 1%、 移動相B: 10% → 99%
30−40分
移動相A:1%、 移動相B: 99%
The content of the acylated sterol glycoside in the rice bran extract used in the present invention can be measured by the following method.
(1) Weigh a suitable amount of rice bran extract, add chloroform / methanol mixture (chloroform: methanol = 2: 1), and measure up in a measuring flask.
(2) The solution obtained in (1) is appropriately diluted according to the component concentration to obtain a sample solution for analysis.
(3) Established Stylyl Glucoside is used as a sample, and the concentration of the acylated sterol glycoside is calculated by high performance liquid chromatography.
(4) Analysis conditions by high performance liquid chromatography method Analyzer: HPLC
Mobile phase A: methanol: water = 95: 5 (v / v)
Mobile phase B: chloroform = 100 (v / v)
Pump: Model 582
solvent delivery system
Analytical column: LiChrosphere Si60 (5 μm)
HPLC-Cartridge (MERCK)
Detector: Charged particle detector (Corona Dionex)
Injection Volume: 20μL
Column oven: 40 ° C. (FLO model 502)
Analysis time: 40 min
Defoaming device: uniflows Degas Ultimate
DV3003
Flow rate: 1 mL / min
Gradient conditions 0-15 minutes as shown below Mobile phase A: 1% → 25%, mobile phase B: 99% → 75%
15-20 minutes Mobile phase A: 25% → 90%, mobile phase B: 75% → 10%
20-25 minutes Mobile phase A: 90%, Mobile phase B: 10%
25-30 minutes Mobile phase A: 90% → 1%, Mobile phase B: 10% → 99%
30-40 minutes Mobile phase A: 1%, Mobile phase B: 99%
本発明に用いられる米糠抽出物は、γ−オリザノールを1.4〜2.1質量%含有する。
γ−オリザノールは、米糠の脂質に含有されるフェルラ酸とステロールのエステルを意味し、フェルラ酸24−メチレンシクロアルテニル、フェルラ酸シクロアルテニル、フェルラ酸カンペステリル、フェルラ酸β−シトステリル等の混合物である。
The rice bran extract used in the present invention contains 1.4 to 2.1% by mass of γ-oryzanol.
γ-Oryzanol means an ester of ferulic acid and sterol contained in rice bran lipid, and is a mixture of 24-methylenecycloartenyl ferulate, cycloartenyl ferulate, campesteryl ferulate, β-sitosteryl ferulate and the like. is there.
本発明に用いられる米糠抽出物中のγ−オリザノールの含有量は、高速液体クロマトグラフィーにて、逆相カラムを用い、紫外線検出器で検出することができる。 The content of γ-oryzanol in the rice bran extract used in the present invention can be detected by high performance liquid chromatography using a reverse phase column and an ultraviolet detector.
本発明に用いられる米糠抽出物は、ステアロ・オレオ・レシチン(ステアロイルオレオイルホスファチジルコリン)換算でリン脂質を18〜28質量%含有する。 The rice bran extract used in the present invention contains 18 to 28% by mass of phospholipid in terms of stearo-oleo-lecithin (stearoyl oleoylphosphatidylcholine).
本発明に用いられる米糠抽出物中のリン脂質の含量はモリブデンブルー吸光光度法により、リンの濃度を測定し、ステアロ・オレオ・レシチン量に換算して求めることができる。具体的には、米糠抽出物からFolch法で脂質を抽出し、灰化後、モリブデンブルー吸光光度法により、リンの濃度を測定する。 The phospholipid content in the rice bran extract used in the present invention can be determined by measuring the phosphorus concentration by molybdenum blue absorptiometry and converting it to the amount of stearo-oleo-lecithin. Specifically, lipid is extracted from the rice bran extract by the Folch method, and after ashing, the phosphorus concentration is measured by molybdenum blue absorptiometry.
本発明に用いられる米糠抽出物は、加水分解したときに、加水分解前の質量に対して20〜30質量%のリノール酸、24〜37質量%のオレイン酸、11〜17質量%のパルミチン酸を含有する。 The rice bran extract used in the present invention, when hydrolyzed, is 20-30% by mass of linoleic acid, 24-37% by mass of oleic acid, 11-17% by mass of palmitic acid with respect to the mass before hydrolysis. Containing.
加水分解後のリノール酸、オレイン酸、パルミチン酸の量は、以下の方法により測定できる。米糠抽出物に0.5mol/L水酸化ナトリウムのメタノール溶液を加えてケン化し、三フッ化ホウ素メタノール錯体メタノール溶液を添加してメチルエステル化する。ヘキサンと飽和食塩水を加えて脂肪酸のメチルエステル化物を分配抽出し、ガスクロマトグラフィーで水素炎イオン検出器を用いて定量分析することができる。 The amount of linoleic acid, oleic acid and palmitic acid after hydrolysis can be measured by the following method. The rice bran extract is saponified by adding a methanol solution of 0.5 mol / L sodium hydroxide, and methyl esterified by adding a boron trifluoride methanol complex methanol solution. Hexane and saturated saline are added to extract and methylate the fatty acid methyl ester, and quantitative analysis can be performed by gas chromatography using a flame ion detector.
本発明に用いられる米糠抽出物は、加水分解したときに、加水分解前の質量に対してアシル化ステロールに由来する1.7〜2.6質量%の植物ステロールを含有する。植物ステロールの主成分は、β−シトステロール、スチグマステロール、カンペステロールである。 The rice bran extract used in the present invention contains 1.7 to 2.6% by mass of plant sterols derived from acylated sterols based on the mass before hydrolysis when hydrolyzed. The main components of plant sterol are β-sitosterol, stigmasterol, and campesterol.
加水分解後の植物ステロールの量は、以下の方法により測定できる。米糠抽出物に塩化ナトリウム水溶液、ピロガロール−エタノール溶液、水酸化カリウム水溶液、水酸化カリウムを順次加えて、ケン化する。塩化ナトリウム水溶液とヘキサン、酢酸エチル混液を添加して、不ケン化物を分配抽出する。不ケン化物からシリカカートリッジカラムを用いて植物ステロール画分を分離し、植物ステロール画分中の植物ステロールをガスクロマトグラフィーで水素炎イオン検出器を用いて定量分析する。 The amount of plant sterol after hydrolysis can be measured by the following method. A saponification is performed by sequentially adding a sodium chloride aqueous solution, a pyrogallol-ethanol solution, a potassium hydroxide aqueous solution, and potassium hydroxide to the rice bran extract. An aqueous sodium chloride solution, hexane and ethyl acetate are added to partition and extract the unsaponifiable matter. The plant sterol fraction is separated from the unsaponifiable matter using a silica cartridge column, and the plant sterol fraction in the plant sterol fraction is quantitatively analyzed by gas chromatography using a flame ion detector.
本発明に用いられる米糠抽出物の抽出方法としては、溶媒抽出法、超臨界抽出法、カラムクロマトグラフィー等が挙げられる。
また、具体的な抽出操作を以下に示す。
Examples of the method for extracting rice bran extract used in the present invention include a solvent extraction method, a supercritical extraction method, and column chromatography.
A specific extraction operation is shown below.
<抽出方法>
市場に流通している米糠を選別した後に、ノルマルヘキサンなどの溶媒を用いて脱脂する。得られた油、脱脂糠等の粗原料を蒸留装置により脱溶媒し、さらにノルマルヘキサン、アセトン、エタノール、水などの溶媒によって抽出する。かくして得られた抽出液を、脱溶剤装置を用いて再度脱溶剤することで米糠抽出物を得ることができる。
<Extraction method>
After selecting rice bran in the market, it is degreased using a solvent such as normal hexane. The obtained crude raw materials such as oil and defatted lees are desolvated with a distillation apparatus, and further extracted with a solvent such as normal hexane, acetone, ethanol, water and the like. The rice bran extract can be obtained by removing the solvent from the extract thus obtained again using a solvent removal apparatus.
前記の米糠抽出物に10質量%以下のワックス類を配合することによって、粉体を混合したときに、粉体は米糠抽出物中に均一な分散状態を維持することが可能となり、有効成分の配合濃度を維持しながらカプセルに充填することができる。なお本発明の組成物を内包するカプセルは公知のカプセルであればどのようなカプセル外殻であっても適用可能であるが、好ましくはゼラチンを主原料とするソフトカプセルが好ましい。 By blending 10% by weight or less of waxes with the rice bran extract, when the powder is mixed, the powder can maintain a uniform dispersion state in the rice bran extract. Capsules can be filled while maintaining the blending concentration. The capsule containing the composition of the present invention can be applied to any capsule outer shell as long as it is a known capsule, but a soft capsule mainly made of gelatin is preferable.
米糠抽出物に配合するワックス類としては、ミツロウ、グリセリン脂肪酸エステル、ショ糖脂肪酸エステル、レシチンなどが挙げられる。 Examples of waxes to be added to the rice bran extract include beeswax, glycerin fatty acid ester, sucrose fatty acid ester, and lecithin.
本発明に用いる粉体としては、βクリプトキサンチン、糖転移ヘスペリジン、コエンザイムQ10、α−リポ酸、GABA、ビタミン類、ミネラル類、アミノ酸、いちょう葉、ヒアルロン酸、コラーゲン、ヒハツエキス、ビルベリーエキス、ショウガエキス、乳酸菌末、食物繊維、納豆菌培養エキス末、紅麹末、ウコンエキス、大豆イソフラボン、大豆サポニン、マリアアザミエキスなどが挙げられる。 Examples of the powder used in the present invention include β cryptoxanthin, transglycosyl hesperidin, coenzyme Q10, α-lipoic acid, GABA, vitamins, minerals, amino acids, ginkgo biloba, hyaluronic acid, collagen, hihatsu extract, bilberry extract, ginger extract. Lactic acid bacteria powder, dietary fiber, natto bacteria extract powder, red yeast rice powder, turmeric extract, soybean isoflavone, soybean saponin, maria thistle extract and the like.
本発明に用いるカプセルとしては、ゼラチン、グリセリン等を組合わせた皮膜が一般的である。カプセル被膜に配合できる他の成分として、カラメル、カラギーナン、寒天、アルギン酸、ペクチン、セルロース誘導体、セルロース、デキストリン、リン酸ナトリウム、デンプン、ソルビトール、トレハロース等の糖質などが挙げられる。 As the capsule used in the present invention, a film combining gelatin, glycerin and the like is generally used. Examples of other components that can be blended in the capsule film include caramel, carrageenan, agar, alginic acid, pectin, cellulose derivatives, saccharides such as cellulose, dextrin, sodium phosphate, starch, sorbitol, and trehalose.
以下に、参考例、実施例を示し、本発明をさらに詳細に説明する。 Hereinafter, the present invention will be described in more detail with reference examples and examples.
<参考例1:米糠抽出物の調製(溶媒抽出)>
市場に流通している米糠を選別し胚乳や異物を除いた米糠を得た。得られた選別済みの米糠10kgに対して50Lのノルマルヘキサンを用い脱脂した。この脱脂作業を1回繰り返し、脱脂米糠を得た。得られた脱脂米糠から蒸留装置により溶媒を除去した。得られた脱脂米糠8kgに対し、50Lの割合でエタノールを用いて70±3℃にて1時間還流しながら抽出した。これを3回繰り返し、得られた抽出液について、脱溶剤装置を用いてエタノールを除去した。米糠抽出物中のアシル化ステロール配糖体、γ−オリザノール、ステアロ・オレオ・レシチン換算のリン脂質の濃度並びに、加水分解前の質量に対する、加水分解後のリノール酸、オレイン酸、パルミチン酸、植物ステロールの濃度を表1に示す。
<Reference Example 1: Preparation of rice bran extract (solvent extraction)>
The rice bran that was distributed in the market was selected to obtain the rice bran from which endosperm and foreign matter were removed. 50 L of normal hexane was used to degrease 10 kg of the obtained sorted rice bran. This degreasing operation was repeated once to obtain a defatted rice bran. The solvent was removed from the resulting defatted rice bran with a distillation apparatus. The obtained defatted rice bran 8 kg was extracted with ethanol at a rate of 50 L while refluxing at 70 ± 3 ° C. for 1 hour. This was repeated three times, and ethanol was removed from the resulting extract using a solvent removal apparatus. Acylated sterol glycoside, γ-oryzanol, stearo-oleo-lecithin equivalent phospholipid concentration in rice bran extract and mass before hydrolysis, linoleic acid, oleic acid, palmitic acid, plant after hydrolysis Table 1 shows the sterol concentration.
<参考例2:米糠抽出物の調製(溶媒抽出)>
市場に流通している米糠を選別し胚乳や異物を除いた米糠を得た。得られた選別済みの米糠10kgに対して50Lのノルマルヘキサンを用い脱脂した。この脱脂作業を3回繰り返し、脱脂米糠を得た。得られた脱脂米糠から蒸留装置により溶媒を除去した。得られた脱脂米糠8kgに対し、50Lの割合でアセトンを用いて50±3℃にて1時間還流しながら抽出した。これを3回繰り返し、得られた抽出液について、脱溶剤装置を用いてアセトンを除去した。米糠抽出物中のアシル化ステロール配糖体、γ−オリザノール、ステアロ・オレオ・レシチン換算のリン脂質の濃度並びに、加水分解前の質量に対する、加水分解後のリノール酸、オレイン酸、パルミチン酸、植物ステロールの濃度を表1に示す。
<Reference Example 2: Preparation of rice bran extract (solvent extraction)>
The rice bran that was distributed in the market was selected to obtain the rice bran from which endosperm and foreign matter were removed. 50 L of normal hexane was used to degrease 10 kg of the obtained sorted rice bran. This degreasing operation was repeated three times to obtain a defatted rice bran. The solvent was removed from the resulting defatted rice bran with a distillation apparatus. The obtained defatted rice bran 8 kg was extracted while refluxing at 50 ± 3 ° C. for 1 hour using acetone at a rate of 50 L. This was repeated three times, and acetone was removed from the resulting extract using a solvent removal apparatus. Acylated sterol glycoside, γ-oryzanol, stearo-oleo-lecithin equivalent phospholipid concentration in rice bran extract and mass before hydrolysis, linoleic acid, oleic acid, palmitic acid, plant after hydrolysis Table 1 shows the sterol concentration.
<粉体混合安定性試験>
粉体としてβクリプトキサンチンを15質量%配合した米糠抽出物を調製し、粉体の分散安定性を確認した。
表2の処方の通り、各原料を秤量後、70℃以上で加温溶解・撹拌し、均一になったのちに、直径10mmのマイクロチューブに1.0ml分注した。
マイクロチューブを40℃条件下に1日静置し、油分と固形分の分離の様子を目視観察した。均一に混合しているものを「○」、分離傾向が見られたものを「△」、分離したものを「×」と評価した。
<Powder mixing stability test>
A rice bran extract containing 15% by mass of β cryptoxanthin was prepared as a powder, and the dispersion stability of the powder was confirmed.
As shown in Table 2, each raw material was weighed and then heated and dissolved and stirred at 70 ° C. or higher. After becoming uniform, 1.0 ml was dispensed into a 10 mm diameter microtube.
The microtube was allowed to stand at 40 ° C. for one day, and the state of separation of oil and solid was visually observed. The samples that were uniformly mixed were evaluated as “◯”, those that showed a separation tendency were evaluated as “Δ”, and those that were separated were evaluated as “×”.
参考例1の米糠抽出物を用いた実施例1、実施例2の組成物は、紛体のβクリプトキサンチンを安定に分散することができた。一方参考例2の米糠抽出物を用いた比較例1,2の粗組成物はβクリプトキサンチンの粉末を安定に分散させることができなかった。
したがって、参考例1の米糠抽出物とミツロウの組み合わせは、カプセルに均一な組成で粉体を分散させた液体を充填する目的に適していることが明らかとなった。
なお、ミツロウの配合量を10%を超えて配合させた場合は、カプセルへの充填に際し、粘度が高くなりすぎて不適であった。
The compositions of Example 1 and Example 2 using the rice bran extract of Reference Example 1 were able to stably disperse powdered β-cryptoxanthin. On the other hand, the crude compositions of Comparative Examples 1 and 2 using the rice bran extract of Reference Example 2 could not stably disperse β cryptoxanthin powder.
Therefore, it was revealed that the combination of the rice bran extract and beeswax of Reference Example 1 is suitable for the purpose of filling the capsule with a liquid in which the powder is dispersed with a uniform composition.
When the amount of beeswax was over 10%, the viscosity was too high when filling the capsule, which was inappropriate.
Claims (4)
ワックス類と
粉体を
含有することを特徴とするカプセル充填用の組成物。 2.7-4.1% by mass of acylated sterol glycoside, 1.4-2.1% by mass of γ-oryzanol, 18-28% by mass of phospholipid in terms of stearo-oleo-lecithin, When hydrolyzed, 20-30% by weight linoleic acid, 24-37% by weight oleic acid, 11-17% by weight palmitic acid, 1.7-2.6% by weight with respect to the weight before hydrolysis. A capsule filling composition comprising a rice bran extract containing a plant sterol, a wax and a powder.
The capsule formulation which includes the composition in any one of Claims 1-3.
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