JP5740530B2 - ペクチンの抽出方法 - Google Patents
ペクチンの抽出方法 Download PDFInfo
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- JP5740530B2 JP5740530B2 JP2014513950A JP2014513950A JP5740530B2 JP 5740530 B2 JP5740530 B2 JP 5740530B2 JP 2014513950 A JP2014513950 A JP 2014513950A JP 2014513950 A JP2014513950 A JP 2014513950A JP 5740530 B2 JP5740530 B2 JP 5740530B2
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- 239000001814 pectin Substances 0.000 title claims description 172
- 229920001277 pectin Polymers 0.000 title claims description 172
- 235000010987 pectin Nutrition 0.000 title claims description 172
- 238000000605 extraction Methods 0.000 title claims description 47
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 121
- 239000000203 mixture Substances 0.000 claims description 68
- 238000000034 method Methods 0.000 claims description 53
- 235000006408 oxalic acid Nutrition 0.000 claims description 33
- 239000011575 calcium Substances 0.000 claims description 22
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 21
- 229910052791 calcium Inorganic materials 0.000 claims description 17
- 235000013399 edible fruits Nutrition 0.000 claims description 17
- 230000032050 esterification Effects 0.000 claims description 17
- 238000005886 esterification reaction Methods 0.000 claims description 17
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 36
- 239000000523 sample Substances 0.000 description 31
- 239000000463 material Substances 0.000 description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
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- 241000196324 Embryophyta Species 0.000 description 23
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- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical group C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
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- PYMYPHUHKUWMLA-UHFFFAOYSA-N 2,3,4,5-tetrahydroxypentanal Chemical compound OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- SATHPVQTSSUFFW-UHFFFAOYSA-N 4-[6-[(3,5-dihydroxy-4-methoxyoxan-2-yl)oxymethyl]-3,5-dihydroxy-4-methoxyoxan-2-yl]oxy-2-(hydroxymethyl)-6-methyloxane-3,5-diol Chemical compound OC1C(OC)C(O)COC1OCC1C(O)C(OC)C(O)C(OC2C(C(CO)OC(C)C2O)O)O1 SATHPVQTSSUFFW-UHFFFAOYSA-N 0.000 description 1
- 229920000189 Arabinogalactan Polymers 0.000 description 1
- 239000001904 Arabinogalactan Substances 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 240000000560 Citrus x paradisi Species 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 244000141359 Malus pumila Species 0.000 description 1
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- 235000019312 arabinogalactan Nutrition 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 1
- 239000001527 calcium lactate Substances 0.000 description 1
- 229960002401 calcium lactate Drugs 0.000 description 1
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- 230000015556 catabolic process Effects 0.000 description 1
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- 230000029087 digestion Effects 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 230000008020 evaporation Effects 0.000 description 1
- 208000006047 familial isolated pituitary adenoma Diseases 0.000 description 1
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical group COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
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- 208000036974 gastrointestinal defects and immunodeficiency syndrome 1 Diseases 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 238000002356 laser light scattering Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
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- 239000008239 natural water Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000010178 pectin extract Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000010318 polygalacturonic acid Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Description
YP%=0.1・yS・M/WP
ここで、YPは、%で示される皮あたりの収率、ySは、g/kgで示される溶液(抽出液)の収率、Mは、ろ過直前の抽出混合物の総質量、WPは、抽出混合物に用いた皮の重量である。当業者に理解されるように、上記の皮あたりの収率の算出は、抽出混合物の総質量のうち少量は溶解しないという点を無視しており、したがって、溶解ペクチンが分布していない量を表すため、近似にすぎない。
フェノールフタレン指示薬を5滴、試料に加え、色の変化が観測されるまで0.1M NaOHで滴定した。20.0mLの0.5M NaOHを、厳密に15分間、攪拌しながら、ホイルで覆われた状態で加えた。そして、色がなくなるまで攪拌しながら20.0mLの0.5M HClを加えた。それから、フェノールフタレン指示薬を3滴加え、色の変化が観測されるまで0.1M NaOHで滴定した(V2力価として記録した)。20mLの0.5M NaOH及びHCl2つの各部分のバランスに生じうる誤差を補償するために、いわゆる「ブラインド測定」を行った(すなわち、100mLの脱イオン水に対して、試料溶液と同様の滴定等の処理を行った)。最終的な滴定結果をB1力価として記録した。それから、以下の計算式によって、エステル化度を表した。
Vt=V1+(V2−B1)
%DE(エステル化度)=[(V2−B1)/Vt]*100
c†=c1+(c2−c1)・(ln(25/η1))/(ln(η2/η1))
M=1+20+0.03+0.0029+0.400+20kg=41.4kg.
WP=1kg.
YP%=0.1・5.71・41.4/1=23.6
M=30+1+0.015+0.050+0.4+10=41.5
YP=24.7.
DE及びIVはいずれも、上述したプロトコルと同じものを用いて計測した。ペクチンは、DE=74.6及びIV=6.59dL/gを有した。収率と固有粘度との積は163であった(実施例1の88%にすぎない)。YogSimBufは3.24g/Lと算出された。これは、従来方法を用いて抽出したペクチンの強度が実施例1で抽出したペクチンの強度の77%にすぎないことを示唆している(なお、「小さい」と「強度が高い」ことに留意されたい)。
Claims (20)
- 果物の皮からペクチンを抽出する方法であって、
果物の皮の水性懸濁液に、シュウ酸及び/又は水溶性シュウ酸塩を、pHが3.0〜3.6であり、シュウ酸塩の全モル濃度が前記果物の皮中のカルシウム(II)の全モル濃度より高い混合物を得るのに十分な量で加えるステップと、
前記混合物を、0.5〜5時間、50℃〜80℃の温度まで加熱するステップと、
前記混合物から前記抽出ペクチンを沈殿させて、当該混合物から当該抽出ペクチンを分離するステップと
を含み、
前記抽出ペクチンは、エステル化度(DE)が72以上であり、6.0dL/g超の固有粘度により特徴付けられるペクチンである、方法。 - 前記混合物から前記抽出ペクチンを分離する前記ステップの前の当該混合物のpHは、3.1〜3.4である、請求項1記載の方法。
- 混合物を加熱する前記ステップ中、前記混合物を、70℃〜80℃の温度まで加熱する、請求項2記載の方法。
- 前記ペクチン抽出する前記ステップの後かつ前記抽出ペクチンを分離する前記ステップの前に、前記混合物をろ過して、不溶性固形物を除去するステップをさらに含む、請求項1記載の方法。
- 前記抽出ペクチンを分離する前記ステップの前に、当該抽出ペクチンを含む前記混合物をイオン交換樹脂と接触させるステップをさらに含む、請求項1記載の方法。
- 前記イオン交換樹脂は、シュウ酸塩、カルシウム塩又はそれらの組み合わせを、前記抽出ペクチンから除去するのに有効な陽イオン交換樹脂を含む、請求項5記載の方法。
- 前記抽出ペクチンの総シュウ酸塩含有量は、ペクチン1gあたり2.0mg未満である、請求項5記載の方法。
- 前記抽出ペクチンの総カルシウム含有量は、1mg/g未満である、請求項5記載の方法。
- 前記抽出ペクチンを分離する前記ステップの後に、当該抽出ペクチンを洗浄、圧搾、乾燥及び粉砕するステップのうち1つ又は複数のステップをさらに含み、最終ペクチン生成物を得る、請求項1記載の方法。
- 果物の皮あたりの収率(YP)は23%超で、YP=0.1・yS・M/WPであり、ここで、ySは、g/kgで示される溶液(抽出液)の収率、Mは、前記抽出ペクチンを分離する前記ステップの前の前記混合物の総質量、WPは、前記水性懸濁液に用いられる前記果物の皮の重量である、請求項1記載の方法。
- 果物の皮あたりの前記収率と前記固有粘度との積は、165%・dL/g超である、請求項10記載の方法。
- 前記抽出ペクチンのエステル化度(DE)は、75以上である、請求項1記載の方法。
- 前記抽出ペクチンの固有粘度(IV)は、7.8dL/g以上である、請求項1記載の方法。
- 前記抽出ペクチンの固有粘度(IV)は、8.5dL/g以上である、請求項1記載の方法。
- 果物の皮からペクチンを抽出する方法であって、
果物の皮の水性懸濁液に、シュウ酸及び/又は水溶性シュウ酸塩を、pHが3.0〜3.6であり、シュウ酸塩の全モル濃度が前記果物の皮中のカルシウム(II)の全モル濃度より高い混合物を得るのに十分な量で加えるステップと、
前記混合物を、0.5〜5時間、50℃〜80℃の温度まで加熱するステップと、
任意選択的に、前記混合物をろ過して、不溶性固形物を除去するステップと、
当該抽出ペクチンを含む前記混合物を陽イオン交換樹脂と接触させるステップと、
前記混合物から前記抽出ペクチンを沈殿させて、当該混合物から当該抽出ペクチンを分離して、23%超の果物の皮あたりの収率(YP)、ここで、YP=0.1・yS・M/WPで、ySは、g/kgで示される溶液(抽出液)の収率、Mは、前記抽出ペクチンを分離する前記ステップの前の前記混合物の総質量、WPは、前記水性懸濁液に用いられる前記果物の皮の重量である、を得るステップと
から実質的に成り、
前記抽出ペクチンは、エステル化度(DE)が72以上であり、6.0dL/g超の固有粘度数により特徴付けられるペクチンである、方法。 - 前記抽出ペクチンの総シュウ酸塩含有量は、ペクチン1gあたり2.0mg未満である、請求項15記載の方法。
- 前記抽出ペクチンの総カルシウム含有量は、1mg/g未満である、請求項15記載の方法。
- 前記混合物を加熱する前記ステップ中、前記混合物を、1時間〜3時間加熱する、請求項15記載の方法。
- 前記抽出ペクチンのエステル化度(DE)は、75以上である、請求項15記載の方法。
- 前記抽出ペクチンの固有粘度(IV)は、7.8dL/g以上である、請求項15記載の方法。
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