JP5579578B2 - 微結晶質セルロース組成物 - Google Patents
微結晶質セルロース組成物 Download PDFInfo
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- JP5579578B2 JP5579578B2 JP2010252690A JP2010252690A JP5579578B2 JP 5579578 B2 JP5579578 B2 JP 5579578B2 JP 2010252690 A JP2010252690 A JP 2010252690A JP 2010252690 A JP2010252690 A JP 2010252690A JP 5579578 B2 JP5579578 B2 JP 5579578B2
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- Prior art keywords
- microcrystalline cellulose
- hydrocolloid
- mcc
- composition
- particle size
- 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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Description
(a)加水分解したセルロースのみを摩擦にかけてコロイド状微結晶質セルロースを製造する工程、
(b)該コロイド状微結晶質セルロースを水中に分散し、乾燥イオータカラギーナンの溶解温度より高い温度に加熱して該コロイド状微結晶質セルロースと共処理する工程、
(c)乾燥イオータカラギーナンをコロイド状微結晶質セルロースの加熱した分散物に添加し、成分を混合してスラリーを生成する工程、
(d)該スラリーをホモゲナイズする工程、そして
(e)該スラリーを乾燥して共処理した粉末を生成する工程。
(a)磨砕されていない微結晶質セルロース、水に比較的不溶な磨砕剤及び所望により保護的コロイドをともにブレンドする工程、
(b)微結晶質セルロースの粒子径を減少させるのに充分な時間及びせん断力の下ブレンドを高いせん断含湿粉砕にかける工程、そして
(c)得られた超微細微結晶質セルロース組成物を回収する工程。
(i)ヒドロコロイドがカラギーナンのとき、粒子の少なくとも約50%が約3.5ミクロンより小さい粒子径を有し、
(ii)ヒドロコロイドがカラギーナン以外のヒドロコロイドであるとき、粒子の少なくとも約30%が約3.5ミクロンより小さい粒子径を有し、そして
(iii)ヒドロコロイドがカラギーナンと他のヒドロコロイドとの混合物であるとき、粒子の少なくとも約20%が約3.5ミクロンより小さい粒子径を有する。
実施例では、以下の標準材料及びテスト法を使用した。
分散物を、Waring Blender(700シリーズ)により、跳ね返しをさけるためにWaring Blenderの速度を次第に上げることを可能にするPowerstat変圧器によってコントロールされる18000−19000rpmの速度で1000mLのボウルを使用して製造した。
(1)秤で16g(±0.01g)を測りとる。
(2)500mLのメスシリンダーで587±1gの蒸留水または脱イオン水を測りとりそしてそれをブレンダーボウル中に注ぐ。
(3)ブレンダーの速度を変圧器により徐々に約30ボルトに上げる。ボウルの側面に付着にしないように注意しつつ、粉末を水の中心に加える。
(4)粉末の添加後、ボウルの蓋をかぶせ15秒間混合する。
(5)15秒混合後、可能な限り早く電圧を115に上げ、そして2分間115ボルトで混合する。
(6)分散物を500mLのNalgene瓶に貯蔵する。
(以下のカルシウムフレーム原子吸収テスト法により測定)
方法
A.標準/ブランク調製
1.以下のように、5%塩化ランタン溶液をつくる
12.5gの塩化ランタン7水和物を正確に測りとり、約100mLの0.1N塩酸(HCl)を含む250mLのメスフラスコに移す。10分間超音波浴におき、取り出し、そして室温に冷却し、次に0.1N HClを満たす。
10.0mLの市販の1000ppmのカルシウム標準品(Thermo Orion No.922006、VWR No.34183−182)を、約50mLの0.1N HClを含む100mLのメスフラスコに移し、充分に振盪し、そして0.1N HClを満たす。
100ppmのカルシウム標準品2、4、7、10、13及び16mLを、10mLの5%塩化ランタン溶液及び約50mLの0.1N HClを含むラベルした100mLのメスフラスコに入れる。充分に振盪し、そして0.1N HClにより満たす。
10mLの5%塩化ランタン溶液を100mLのメスフラスコの入れ、そして0.1N HClを満たす。
B.サンプルの調製
1.水分%を測定するためにすべてのサンプルについて乾燥損失(LOD)テストを行う。
3.30分間超音波浴におき、取り出し、そして室温に冷却する。
4.10mLの5%塩化ランタン溶液を添加し、0.1N HClを満たす。
5.3500rpm/5分間で遠心分離し、そして上清を13×100mmの管に入れる。
6.必要に応じ0.5%塩化ランタンを含む0.1N HClにより希釈して、標準曲線の2−16ppmのカルシウム範囲内の結果を達成する。
装置:Perkin−Elmer Analyst 300原子吸収分光計
ランプ:カルシウム
波長:422.8nm
シグナル測定:時間平均
フレームタイプ:空気/アセチレン
オキシダント流:10.0L/分
燃料流:3.0L/分
スリット幅:0.7
読み取り時間:5秒
遅延時間:28秒
較正:線形
カルシウムの重量(mg)=ppmカルシウム・100・希釈ファクター/1000
%カルシウム=(カルシウムの重量(mg)/サンプル重量(mg)・(100−%LOD/100))・100
%塩化カルシウム=%カルシウム・(110.98/40.08)
ベーキング安定性は、以下の方法により形状保持を測定することによって測定された。形状保持は、所定の温度で或る時間焼かれた後その最初の形状及び体積を保持するフルーツのフィリングの製品の能力として定義される。或る体積のフルーツのフィリングの製品(約35g)を標準化したリング(3.5cm)にいれ、それを同心円の目盛をつけた紙におく。フルーツのフィリングを、通風オーブンで特定の温度で或る時間(通常華氏400度で10分間)焼く。熱処理後、フルーツのフィリングの広がりを測定する。広がりは、%[(最後の直径−最初の直径)/最初の直径×100]で表示される。
〔実施例〕
(抗スリップ剤なし)
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1744.9gの微結晶質セルロース(MCC)を、90.8gのイオータカラギーナンと混合して90/10重量部のMCC対イオータカラギーナン固体比を得た。混合物を数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは非常に滑りやすく、そのためMCC凝集物を機械的に崩壊させてコロイド状粒子を生成するのに必要な摩擦または押し出し機の作業プロフィルは得られなかった。押し出し物の顕微鏡的評価は、MCC粒子が大きくしかも磨砕されておらず、従ってそれらがコロイド状でないことを明らかにした。
(不十分なレベルの抗スリップ剤)
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1539.3gの微結晶質セルロース(MCC)を、127.8gのイオータカラギーナンと混合して90/10重量部のMCC対イオータカラギーナン固体比を得た。25.0gの30%CaCl2溶液を添加し、そして数分間混合した。混合物を数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは非常に滑りやすく、そのためMCC凝集物を機械的に崩壊させて超微細粒子にするのに必要な摩擦または押し出し機の作業プロフィルは得られなかった。押し出し物の顕微鏡的評価は、MCC粒子が大きくしかも磨砕されておらず、従ってそれらがコロイド状でないことを明らかにした。添加されたカルシウム塩の量は、水についてカラギーナンと競合し、カラギーナンガムをさらに溶媒和するのに不十分であった。
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1938.1gの微結晶質セルロース(MCC)ウエットケーキを、168.9gの完全に変性したカルシウムカッパカラギーナンと混合して望ましいMCC対カッパカラギーナンの固体比を得た。100gの15%CaCl2溶液を添加し、そして数分間混合した。混合物を、数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは、滑ることがなく、それによりコロイド状の微結晶質セルロース粒子の形成を助ける高い作業プロフィルにかけることができた。
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1676.5gの微結晶質セルロース(MCC)ウエットケーキを、100gの30%CaCl2溶液を添加し、そして数分間混合した。324.1gの高メトキシル(HM)ペクチンを添加して所望のMCC対HMペクチン固体比を得た。混合物を、数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは、滑ることがなく、それによりコロイド状の微結晶質セルロース粒子の形成を助ける高い作業プロフィルにかけることができた。
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1089.8gの微結晶質セルロース(MCC)ウエットケーキを、197.2gの高度のエステル化度(DE)を有するプロピレングリコールアルギネート(PGA)と混合して望ましいMCC対PGAの固体比を得た。65gの30%CaCl2溶液を添加し、そして数分間混合した。混合物を、数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは、滑ることがなく、それによりコロイド状の微結晶質セルロース粒子の形成を助ける高い作業プロフィルにかけることができた。312.0gのMCC/PGA押し出し物を、華氏約160度で2268.9gの蒸留水に分散した。1.35gのK2CO3を添加し、そして数分間混合してpHを8.0−8.5に調節した。得られるスラリーを、2500psiでManton Gaulinホモゲナイザーを通し、噴霧乾燥して粉末を形成させた。噴霧乾燥は以下のように行われた。ホモゲナイズしたスラリーを、ノズル噴霧化0.1インチ(0.00254m)開口を利用して3フィート(0.9144m)のBowen噴霧乾燥機に供給した。スラリーを、所望の出口温度を生ずる速度で可変供給Moynoポンプによって乾燥機に供給した。噴霧乾燥機の操作入口/出口の空気温度は、約195℃/95℃であった。噴霧乾燥条件は、供給物の性質例えば粘度、得られる乾燥生成物の特徴及び結果として生ずる収量に応じて調節された。
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1818.8gの微結晶質セルロース(MCC)ウエットケーキを、163.7gのイオータカラギーナンと混合して所望のMCC対イオータカラギーナン固体比を得た。200gの15%CaCl2溶液を添加し、そして数分間混合した。混合物を共回転2軸押し出し機に1回通した。108gの高メトキシル(HM)ペクチンをMCC/イオータカラギーナン混合物に添加した。これを、数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは、滑ることがなく、それによりコロイド状の微結晶質セルロース粒子の形成を助ける高い作業プロフィルにかけることができた。
5ガロンのHobartミキサー中で、38−44%に及ぶ固体含量を有する1818.8gの微結晶質セルロース(MCC)ウエットケーキを、163.7gのイオータカラギーナンと混合して所望のMCC対イオータカラギーナン固体比を得た。200gの15%CaCl2・2H2O溶液を添加し、そして数分間混合した。混合物を共回転2軸押し出し機に1回通した。107.2gのキサンタンガムをMCC/イオータカラギーナン混合物に添加した。これを、数回共回転2軸押し出し機を通して混合物をせん断し、そして微結晶質凝集物を細かく砕いた。押し出し物の得られたコンシステンシーは、滑ることがなく、それによりコロイド状の微結晶質セルロース粒子の形成を助ける高い作業プロフィルにかけることができた。
GRINSTED LA410−Daniscoから入手できる低エステルアミド化ペクチン。
COLFLO 67−National Starchから入手できるワックス状とうもろこしからの変性調理ずみ澱粉。
ラズペリー濃縮物−IFFから入手できる20%フルーツ固体。
MCC/アルギン酸ナトリウム−上記の実施例9で記述したようにして製造。
GRINSTED LA410 5
MCC/アルギン酸ナトリウム 5
水 420
砂糖 337
COLFLO 67澱粉 20
ラズベリー濃縮物 200
ソルビン酸カリウム 1
水中3%乳酸カルシウム 5
水中50%クエン酸 7
ブリックス固体 43%
加熱粘度、cp 13800
ベーキング安定性 11%
ゲル強さ、g 75
(付記1)
(a)少なくとも70重量%の微結晶質セルロース及び(b)ヒドロコロイドからなる組成物であって、約10ミクロンより小さい平均粒子径をもつことを特徴とする組成物。
(付記2)
(i)ヒドロコロイドがカラギーナンであるとき、粒子の少なくとも約50%が約3.5ミクロンより小さい粒子径を有し、
(ii)ヒドロコロイドがカラギーナン以外のヒドロコロイドであるとき、粒子の少なくとも約30%が約3.5ミクロンより小さい粒子径を有し、そして
(iii)ヒドロコロイドがカラギーナンと他のヒドロコロイドとの組み合わせであるとき、粒子の少なくとも約20%が約3.5ミクロンより小さい粒子径を有する
付記1の組成物。
(付記3)
組成物の全重量に基づいて0.18−3.5重量%のCa++含量を有する付記1の組成物。
(付記4)
ヒドロコロイドの量が、ヒドロコロイドと微結晶質セルロースとの全重量に基づいて15−30重量%に等しい付記1の組成物。
(付記5)
ヒドロコロイドがカラギーナンである付記1の組成物。
(付記6)
ヒドロコロイドがアルギネートである付記1の組成物。
(付記7)
微結晶質セルロースの量が、ヒドロコロイドと微結晶質セルロースとの全重量に基づいて70−85重量%に等しい付記1の組成物。
(付記8)
水溶性無機塩をさらに含む付記1の組成物。
(付記9)
無機塩の量が、組成物の全重量に基づいて少なくとも1重量%に等しい付記8の組成物。
(付記10)
無機塩が、塩化ナトリウム、塩化カルシウム、乳酸カルシウム、酒石酸カルシウム及びモノ燐酸カルシウムからなる群から選ばれる付記7の組成物。
(付記11)
無機塩が塩化カルシウムである付記7の組成物。
(付記12)
微結晶質セルロース及びヒドロコロイドがともに磨砕されている付記1の組成物。
(付記13)
微結晶質セルロース組成物を製造する方法であって、
(a)微結晶質セルロース、ヒドロコロイド及び抗スリップ剤の高固体混合物を形成し、
そして
(b)混合物を練合する
ことからなることを特徴とする方法。
(付記14)
微結晶質セルロースが、抗スリップ剤が添加される前にヒドロコロイドと混合される付記13の方法。
(付記15)
微結晶質セルロースが、ヒドロコロイドが添加される前に抗スリップ剤と混合される付記13の方法。
(付記16)
ヒドロコロイドが、カラギーナン及びアルギネートからなる群から選ばれる付記13の方法。
(付記17)
ヒドロコロイドがカラギーナンである付記13の方法。
(付記18)
ヒドロコロイドがアルギネートである付記13の方法。
(付記19)
抗スリップ剤が無機塩の水溶液である付記13の方法。
(付記20)
無機塩が2価の塩である付記19の方法。
(付記21)
2価の塩が塩化カルシウムである付記20の方法。
(付記22)
無機塩の量が、混合物中の固体の全重量に基づいて約0.8−約3.0重量%に等しい付記19の方法。
(付記23)
抗スリップ剤が無機塩である付記17の方法。
(付記24)
無機塩の量が、混合物中の固体の全重量に基づいて1.0−3.0重量%に等しい付記23の方法。
(付記25)
抗スリップ剤が無機塩である付記18の方法。
(付記26)
無機塩の量が、混合物中の固体の全重量に基づいて0.8−2.0重量%に等しい付記25の方法。
(付記27)
付記1の組成物を含むことを特徴とする食品。
(付記28)
付記1の組成物を含むことを特徴とする製薬組成物。
(付記29)
付記1の組成物を含むことを特徴とする化粧品組成物。
(付記30)
付記1の組成物を含むことを特徴とする製薬投与形。
(付記31)
付記1の組成物を含むことを特徴とする工業用組成物。
Claims (5)
- (a)微結晶質セルロース及び(b)カラギーナン以外のヒドロコロイドのみからなる共磨砕された組成物であって、
(i)当該組成物が、6.04ミクロン以上で10ミクロンより小さい平均粒子径を有し、
(ii)粒子の少なくとも30%が3.5ミクロンより小さい粒子径を有し、そして
(iii)当該組成物が、少なくとも70重量%の微結晶質セルロースからなる、共磨砕された組成物。 - (a)微結晶質セルロース、(b)カラギーナン以外のヒドロコロイド、及び(c)抗スリップ剤のみからなる共磨砕された組成物であって、
(i)当該組成物が、6.04ミクロン以上で10ミクロンより小さい平均粒子径を有し、
(ii)粒子の少なくとも30%が3.5ミクロンより小さい粒子径を有し、そして
(iii)当該組成物が、少なくとも70重量%の微結晶質セルロースからなる、共磨砕された組成物。 - ヒドロコロイドの量がヒドロコロイドと微結晶質セルロースとの全重量に基づいて15−30重量%である、請求項1又は2に記載の組成物。
- ヒドロコロイドがセルロースガムからなる請求項1から3のいずれか1項に記載の組成物。
- 2.6%の水分散物において測定したとき、2000cpsの最初の粘度、及び、24時間後に12900cpsの最終粘度を有する、請求項1から4のいずれか1項に記載の組成物。
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US38039802P | 2002-05-14 | 2002-05-14 | |
US60/380,398 | 2002-05-14 |
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- 2003-05-14 WO PCT/US2003/015146 patent/WO2003096976A2/en active Search and Examination
- 2003-05-14 US US10/513,530 patent/US7462232B2/en not_active Expired - Lifetime
- 2003-05-14 JP JP2004504975A patent/JP4808960B2/ja not_active Expired - Fee Related
- 2003-05-14 ES ES03728896T patent/ES2752452T3/es not_active Expired - Lifetime
- 2003-05-14 EP EP03728896.6A patent/EP1575487B1/en not_active Expired - Lifetime
- 2003-05-14 AU AU2003234555A patent/AU2003234555A1/en not_active Abandoned
- 2003-05-14 BR BRPI0309894A patent/BRPI0309894B8/pt not_active IP Right Cessation
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2008
- 2008-11-06 US US12/265,970 patent/US7871468B2/en not_active Expired - Fee Related
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2010
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- 2010-12-20 US US12/972,697 patent/US8801847B2/en not_active Expired - Fee Related
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2014
- 2014-04-23 JP JP2014088780A patent/JP2014185347A/ja active Pending
- 2014-07-10 US US14/327,672 patent/US20140322282A1/en not_active Abandoned
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ES2752452T3 (es) | 2020-04-06 |
JP2006508195A (ja) | 2006-03-09 |
WO2003096976A3 (en) | 2009-04-09 |
JP2011046962A (ja) | 2011-03-10 |
BR0309894A (pt) | 2005-03-22 |
US7462232B2 (en) | 2008-12-09 |
BRPI0309894B1 (pt) | 2019-05-21 |
BRPI0309894B8 (pt) | 2021-07-27 |
EP1575487B1 (en) | 2019-08-14 |
EP1575487A4 (en) | 2012-12-05 |
US20140322282A1 (en) | 2014-10-30 |
US20090130287A1 (en) | 2009-05-21 |
AU2003234555A8 (en) | 2009-05-07 |
JP2014185347A (ja) | 2014-10-02 |
US20060096500A1 (en) | 2006-05-11 |
US8801847B2 (en) | 2014-08-12 |
US20110135798A1 (en) | 2011-06-09 |
CN101404892B (zh) | 2012-04-04 |
WO2003096976A2 (en) | 2003-11-27 |
AU2003234555A1 (en) | 2003-12-02 |
EP1575487A2 (en) | 2005-09-21 |
JP4808960B2 (ja) | 2011-11-02 |
CN101404892A (zh) | 2009-04-08 |
US7871468B2 (en) | 2011-01-18 |
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