JP4772912B1 - Method for producing bleached processed starch - Google Patents
Method for producing bleached processed starch Download PDFInfo
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- JP4772912B1 JP4772912B1 JP2010131976A JP2010131976A JP4772912B1 JP 4772912 B1 JP4772912 B1 JP 4772912B1 JP 2010131976 A JP2010131976 A JP 2010131976A JP 2010131976 A JP2010131976 A JP 2010131976A JP 4772912 B1 JP4772912 B1 JP 4772912B1
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- 229920002472 Starch Polymers 0.000 title claims abstract description 211
- 235000019698 starch Nutrition 0.000 title claims abstract description 210
- 239000008107 starch Substances 0.000 title claims abstract description 208
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 235000013305 food Nutrition 0.000 claims abstract description 35
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 32
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000012545 processing Methods 0.000 claims abstract description 25
- 238000004132 cross linking Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000006640 acetylation reaction Methods 0.000 claims abstract description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000021736 acetylation Effects 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 229920000881 Modified starch Polymers 0.000 claims abstract description 4
- 239000004368 Modified starch Substances 0.000 claims abstract description 4
- 235000019426 modified starch Nutrition 0.000 claims abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 46
- 239000000460 chlorine Substances 0.000 claims description 46
- 229910052801 chlorine Inorganic materials 0.000 claims description 46
- 229920002261 Corn starch Polymers 0.000 claims description 16
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 16
- 239000008120 corn starch Substances 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 13
- 240000003183 Manihot esculenta Species 0.000 claims description 10
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 10
- 238000012790 confirmation Methods 0.000 claims description 6
- 229920001592 potato starch Polymers 0.000 claims description 6
- 244000017020 Ipomoea batatas Species 0.000 claims description 3
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 3
- 235000021067 refined food Nutrition 0.000 claims description 3
- 238000004061 bleaching Methods 0.000 abstract description 32
- 238000012993 chemical processing Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 49
- 239000000725 suspension Substances 0.000 description 47
- 238000011282 treatment Methods 0.000 description 40
- 238000006243 chemical reaction Methods 0.000 description 35
- 239000005708 Sodium hypochlorite Substances 0.000 description 30
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 24
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Substances [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 24
- 239000000523 sample Substances 0.000 description 20
- 239000000126 substance Substances 0.000 description 19
- 239000003795 chemical substances by application Substances 0.000 description 17
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 17
- 235000010262 sodium metabisulphite Nutrition 0.000 description 17
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 15
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 13
- 239000007787 solid Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 239000003513 alkali Substances 0.000 description 11
- 230000002378 acidificating effect Effects 0.000 description 10
- 239000001361 adipic acid Substances 0.000 description 7
- 235000011037 adipic acid Nutrition 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 230000036541 health Effects 0.000 description 6
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 5
- 239000004370 Bleached starch Substances 0.000 description 5
- 235000019428 bleached starch Nutrition 0.000 description 5
- 239000001254 oxidized starch Substances 0.000 description 5
- 235000013808 oxidized starch Nutrition 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 235000009508 confectionery Nutrition 0.000 description 4
- 238000002845 discoloration Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000006174 pH buffer Substances 0.000 description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 4
- 235000015067 sauces Nutrition 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical compound CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- -1 alkenyl succinic acid Chemical compound 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 244000144972 livestock Species 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 235000012149 noodles Nutrition 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000013094 purity test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- UGTZMIPZNRIWHX-UHFFFAOYSA-K sodium trimetaphosphate Chemical compound [Na+].[Na+].[Na+].[O-]P1(=O)OP([O-])(=O)OP([O-])(=O)O1 UGTZMIPZNRIWHX-UHFFFAOYSA-K 0.000 description 2
- 239000001384 succinic acid Substances 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 1
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- 229920000856 Amylose Polymers 0.000 description 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 240000004922 Vigna radiata Species 0.000 description 1
- 235000010721 Vigna radiata var radiata Nutrition 0.000 description 1
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000001073 acetylated oxidized starch Substances 0.000 description 1
- 235000013770 acetylated oxidized starch Nutrition 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000015071 dressings Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 235000015220 hamburgers Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 description 1
- 235000020991 processed meat Nutrition 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229940100486 rice starch Drugs 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000011888 snacks Nutrition 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229940100445 wheat starch Drugs 0.000 description 1
Landscapes
- Grain Derivatives (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
【課題】化学的加工処理が施された加工澱粉において、澱粉の性質を変化させずに十分な漂白効果を得ることが可能な加工澱粉の製造方法の提供。
【解決手段】澱粉を次亜塩素酸またはその塩と反応させた後、食品用加工澱粉を得るための加工処理を行う、漂白された食品用加工澱粉の製造方法であって、食品用加工澱粉を得るための加工処理が、ヒドロキシプロピル化処理、リン酸架橋処理、および酢酸ビニルモノマーを用いたアセチル化処理からなる群から選択される1種または2種以上の加工処理である、製造方法。
【選択図】なし[Problem] To provide a process for producing a modified starch capable of obtaining a sufficient bleaching effect in a modified starch subjected to a chemical processing without changing the properties of the starch.
A method for producing bleached processed starch for food, wherein the starch is reacted with hypochlorous acid or a salt thereof, and then processed to obtain processed starch for food. The manufacturing method in which the processing for obtaining is one or more types of processing selected from the group consisting of hydroxypropylation, phosphoric acid crosslinking, and acetylation using vinyl acetate monomer.
[Selection figure] None
Description
本発明は漂白された加工澱粉の製造方法に関し、より詳細には、次亜塩素酸により漂白された食品用加工澱粉の製造方法に関する。 The present invention relates to a method for producing bleached processed starch, and more particularly to a method for producing processed starch for foods bleached with hypochlorous acid.
澱粉は、コーン、馬鈴薯、キャッサバなどの原料を水溶液中で粗砕きする磨砕工程、外皮などの繊維を除く篩工程、澱粉と蛋白質が含有する懸濁液を両者の比重差によって分離する工程、加工澱粉ならば化学的加工処理の工程、洗浄・脱水する工程、乾燥工程により製造される。この方法により澱粉の純度は99%程度まで高めることが可能となる。しかし、得られた澱粉には微量なタンパク質が残存している。例えば、コーンスターチの場合、0.3%程度のタンパク質が残存しており、上記の方法ではそれ以上の澱粉の精製は困難である。これまでに、澱粉懸濁液中に次亜塩素酸ナトリウムを添加し、タンパク質を酸化、分離する方法が知られており、そのような方法により得られた澱粉は漂白澱粉と呼ばれる。 Starch is a grinding process in which raw materials such as corn, potato and cassava are roughly crushed in an aqueous solution, a sieving process to remove fibers such as hulls, a process in which a suspension containing starch and protein is separated by the difference in specific gravity between the two, Processed starch is produced by chemical processing, washing / dehydration, and drying. By this method, the starch purity can be increased to about 99%. However, a trace amount of protein remains in the obtained starch. For example, in the case of corn starch, about 0.3% of protein remains, and it is difficult to further refine starch by the above method. So far, a method of adding sodium hypochlorite to a starch suspension to oxidize and separate proteins is known, and starch obtained by such a method is called bleached starch.
ところで、加工澱粉は澱粉の構造や性質を変化させるような加工が施された澱粉であり、食品産業や他の様々な産業で利用されている。最も代表的な加工澱粉の一つとして、次亜塩素酸ナトリウムを用いて加工された酸化澱粉がある。酸化澱粉は、次亜塩素酸により澱粉を処理し、澱粉を漂白するとともに、カルボキシル基を導入することにより澱粉の性質を変化させたものである(厚労省食安発第1001001号(平成20年10月1日))。酸化澱粉は粘度が低く、主として製紙工業で用いられている。 By the way, processed starch is starch that has been processed to change the structure and properties of starch, and is used in the food industry and various other industries. One of the most representative processed starches is oxidized starch processed using sodium hypochlorite. Oxidized starch is obtained by treating starch with hypochlorous acid, bleaching the starch, and changing the properties of the starch by introducing carboxyl groups (Ministry of Health, Labor and Welfare, Food Safety No. 1001001 (2008)). October 1 of the year)). Oxidized starch has a low viscosity and is mainly used in the paper industry.
一方、澱粉の構造を変化させずに酸化剤を用いて漂白された澱粉は漂白澱粉と呼ばれ、食品として利用されている。すなわち、漂白澱粉は、澱粉を酸化剤で処理することにより、基本的には、化学的修飾を行うことなく、他の色素成分を酸化等することにより、澱粉の色調を調整したものである(厚労省食安発第1001001号(平成20年10月1日))。澱粉懸濁液中に次亜塩素酸ナトリウムを添加し、タンパク質を酸化、分離して得られた前述の漂白澱粉はその一例である。 On the other hand, starch that has been bleached with an oxidizing agent without changing the structure of the starch is called bleached starch and is used as food. That is, bleached starch is obtained by adjusting the color tone of starch by treating starch with an oxidizing agent, basically oxidizing other pigment components without chemically modifying the starch ( No. 1001001 from the Ministry of Health, Labor and Welfare (October 1, 2008)). One example is the aforementioned bleached starch obtained by adding sodium hypochlorite to the starch suspension to oxidize and separate the protein.
ここで、厚労省食安発第1001001号(平成20年10月1日)によれば、次亜塩素酸ナトリウムを用いて漂白処理を行った澱粉のうち、酸化澱粉の純度試験でカルボキシル基が0.1%を超えるものおよびカルボキシル基が0.1%以下のものであっても、酸化澱粉のカルボキシル基の確認試験の結果が陽性または擬陽性で、かつ、粘度等の澱粉の性質に生じた変化が酸化によるものではないことを合理的に説明できないものについては、澱粉の性質を変化させるほどの化学処理が行われているものと判断し、「漂白澱粉」として取り扱わず、「酸化澱粉」として取り扱うこととされている。また、厚労省食安発第1001001号(平成20年10月1日)によれば、食品用加工澱粉において、酸化との併用が認められている他の化学修飾は、無水酢酸を用いたアセチル化のみである。 Here, according to the Ministry of Health, Labor and Welfare Food Safety No. 1001001 (October 1, 2008), among the starches bleached using sodium hypochlorite, the carboxyl group was tested in the purity test of oxidized starch. Even if the content exceeds 0.1% and the carboxyl group content is 0.1% or less, the result of the confirmation test of the carboxyl group of the oxidized starch is positive or false positive and occurs in the starch properties such as viscosity. If it is not possible to reasonably explain that the change is not due to oxidation, the chemical is judged to have been chemically treated to change the properties of the starch and is not treated as “bleached starch”. It is supposed to be handled as. In addition, according to the Ministry of Health, Labor and Welfare Food Safety No. 1001001 (October 1, 2008), other chemical modifications that are allowed to be combined with oxidation in processed starch for food use acetic anhydride. Only acetylation.
このことから、次亜塩素酸を用いて澱粉を十分に漂白処理すると澱粉の性質が変化する処理が行われたと判断され、更に、化学的な加工処理を施すと二度の加工処理がなされたと判断され、食品用加工澱粉として使用できなくなる。すなわち、所望の化学的な加工処理が施された食品用加工澱粉を提供する場合には次亜塩素酸による十分な漂白処理ができなくなる。従って、化学的な加工処理を施した食品用加工澱粉では、澱粉の性質を変化させずに十分な漂白効果を達成することが必要になる。 From this, it is judged that the starch has been sufficiently bleached using hypochlorous acid, and that the properties of the starch have been changed, and further, the chemical processing has been performed twice. It is judged and cannot be used as processed starch for food. That is, in the case of providing a processed starch for food that has been subjected to a desired chemical processing treatment, a sufficient bleaching treatment with hypochlorous acid cannot be performed. Therefore, processed starch for foods that has been subjected to chemical processing needs to achieve a sufficient bleaching effect without changing the properties of the starch.
特許文献1および特許文献2には、特定条件下で少量の次亜塩素酸ナトリウムを澱粉に添加して、高粘性の澱粉を製造する方法が開示されている。 Patent Document 1 and Patent Document 2 disclose a method for producing a highly viscous starch by adding a small amount of sodium hypochlorite to starch under specific conditions.
特許文献3には、澱粉に多量の次亜塩素酸ナトリウムを添加して酸化処理を行った後にアルカリ処理を行い、その後少量の次亜塩素酸ナトリウムを添加して澱粉を漂白することにより、優れた粘度安定性を有する澱粉を製造する方法が開示されている。 Patent Document 3 is excellent by adding a large amount of sodium hypochlorite to starch and subjecting it to an oxidation treatment and then adding a small amount of sodium hypochlorite to bleach the starch. A method for producing starch having high viscosity stability is disclosed.
特許文献4には、澱粉懸濁液のpHを調整した上で次亜塩素酸ナトリウムを添加して反応を行い、残留塩素臭が少なく、かつ増粘効果が高い澱粉を製造する方法が開示されている。 Patent Document 4 discloses a method for producing starch having a low residual chlorine odor and a high thickening effect by adjusting the pH of the starch suspension and then adding sodium hypochlorite for reaction. ing.
しかしながら、いずれの文献にも、満足な漂白効果が得られ、かつ、化学的な加工処理が施された加工澱粉は開示されていない。 However, none of the documents discloses a modified starch that has a satisfactory bleaching effect and is chemically processed.
本発明は、食品用加工澱粉を得るための加工処理が施された加工澱粉の製造方法において、澱粉の性質を変化させずに十分な漂白効果を得ることが可能な加工澱粉の製造方法を提供することを目的とする。 The present invention provides a method for producing a processed starch capable of obtaining a sufficient bleaching effect without changing the properties of the starch in the method for producing a processed starch that has been processed to obtain a processed starch for food. The purpose is to do.
本発明によれば、澱粉を次亜塩素酸またはその塩と反応させた後、食品用加工澱粉を得るための加工処理を行う、漂白された食品用加工澱粉の製造方法が提供される。この製造方法では、食品用加工澱粉を得るための加工処理は、ヒドロキシプロピル化処理、リン酸架橋処理、および酢酸ビニルモノマーを用いたアセチル化処理からなる群から選択される1種または2種以上の加工処理とされる。 ADVANTAGE OF THE INVENTION According to this invention, after making starch react with hypochlorous acid or its salt, the manufacturing method of the bleached food processed starch which performs the process for obtaining processed food starch is provided. In this production method, the processing for obtaining the processed starch for food is one or more selected from the group consisting of hydroxypropylation, phosphoric acid crosslinking, and acetylation using a vinyl acetate monomer. It is assumed that the processing.
本発明による製造方法により得られた食品用加工澱粉は、従来にない高い白度を有する。従って、本発明による製造方法は、高い白度が求められる食品の製造に用いることができるとともに、漂白処理に用いる薬剤の使用量を低減できる点および有効塩素濃度に由来する塩素臭を低減する点で有利である。 The processed starch for foods obtained by the production method according to the present invention has a high whiteness that has not existed before. Therefore, the production method according to the present invention can be used for the production of foods that require high whiteness, can reduce the amount of chemicals used for bleaching treatment, and can reduce the chlorine odor derived from the effective chlorine concentration. Is advantageous.
本発明による製造方法で出発原料として用いる澱粉は食品用途の澱粉であればいずれも使用できる。食品用途の澱粉としては、例えば、コーンスターチ、ハイアミロースコーンスターチ、ワキシーコーンスターチ、サゴ澱粉、緑豆澱粉、小麦澱粉、米澱粉、馬鈴薯澱粉、甘藷澱粉、タピオカ澱粉が挙げられ、好ましくは、コーンスターチ、ワキシーコーンスターチ、馬鈴薯澱粉、タピオカ澱粉、サゴ澱粉、甘藷澱粉である。 Any starch can be used as a starting material in the production method according to the present invention as long as it is a starch for food use. Examples of starch for food use include corn starch, high amylose corn starch, waxy corn starch, sago starch, mung bean starch, wheat starch, rice starch, potato starch, sweet potato starch, and tapioca starch, preferably corn starch, waxy corn starch, Potato starch, tapioca starch, sago starch and sweet potato starch.
本発明による製造方法では、未処理の澱粉を次亜塩素酸またはその塩で処理する。次亜塩素酸の塩としては次亜塩素酸ナトリウム、次亜塩素酸カリウム、次亜塩素酸カルシウムが挙げられる。 In the production method according to the present invention, untreated starch is treated with hypochlorous acid or a salt thereof. Examples of hypochlorous acid salts include sodium hypochlorite, potassium hypochlorite, and calcium hypochlorite.
澱粉と次亜塩素酸またはその塩との反応は、澱粉の加工処理と判断されないように澱粉の構造や性質を変化させない程度で実施する。具体的には、次亜塩素酸またはその塩と反応させて得られた澱粉中のカルボキシル基含量が0.1質量%未満であり、かつ、該澱粉がカルボキシル基の確認試験で陰性を示すように澱粉と次亜塩素酸塩またはその塩を反応させることができる。 The reaction between starch and hypochlorous acid or a salt thereof is carried out to such an extent that the structure and properties of the starch are not changed so that it is not determined that the starch is processed. Specifically, the carboxyl group content in the starch obtained by reacting with hypochlorous acid or a salt thereof is less than 0.1% by mass, and the starch is negative in the carboxyl group confirmation test. It is possible to react starch with hypochlorite or a salt thereof.
次亜塩素酸またはその塩による処理によって澱粉中に導入されたカルボキシル基の含有量は常法に従って定量することができ、例えば、厚生労働省告示第485号に記載されたアセチル化酸化デンプンのカルボキシル基の純度試験の方法に従って実施することができる。 The content of carboxyl groups introduced into starch by treatment with hypochlorous acid or a salt thereof can be quantified according to a conventional method, for example, carboxyl groups of acetylated oxidized starch described in Ministry of Health, Labor and Welfare Notification No. 485. According to the purity test method.
また、澱粉中に導入されたカルボキシル基の確認試験は、例えば、厚生労働省告示第485号に記載されたアセチル化酸化デンプンのカルボキシル基の確認試験の方法に従って実施することができる。 Moreover, the confirmation test of the carboxyl group introduce | transduced in starch can be implemented according to the method of the confirmation test of the carboxyl group of the acetylation oxidation starch described in Ministry of Health, Labor and Welfare Notification No. 485, for example.
本発明による製造方法では、水に澱粉を懸濁して得られた澱粉懸濁液を反応系に用いることができ、澱粉懸濁液の澱粉濃度は澱粉乾燥質量で20〜45質量%、好ましくは、36〜43質量%とすることができる。また、澱粉乾燥質量に対する有効塩素濃度が200〜5500ppm、好ましくは、500〜3000ppmとなるように次亜塩素酸またはその塩を澱粉懸濁液に添加することができる。この場合、澱粉と次亜塩素酸との反応時間および反応温度は、反応効率の観点から、それぞれ、5〜90分(好ましくは、10〜60分)、20〜55℃(好ましくは、28〜35℃)とすることができる。また、澱粉懸濁液のpHは、反応効率の観点から、3.0〜11.5(好ましくは4.0〜10.5)とすることができる。 In the production method according to the present invention, a starch suspension obtained by suspending starch in water can be used in the reaction system, and the starch concentration of the starch suspension is 20 to 45% by mass in terms of dry starch mass, preferably 36-43 mass%. Hypochlorous acid or a salt thereof can be added to the starch suspension so that the effective chlorine concentration relative to the dry starch mass is 200 to 5500 ppm, preferably 500 to 3000 ppm. In this case, the reaction time and reaction temperature of starch and hypochlorous acid are 5 to 90 minutes (preferably 10 to 60 minutes), 20 to 55 ° C. (preferably 28 to 55 minutes), respectively, from the viewpoint of reaction efficiency. 35 ° C.). The pH of the starch suspension can be set to 3.0 to 11.5 (preferably 4.0 to 10.5) from the viewpoint of reaction efficiency.
本発明による製造方法では、次亜塩素酸またはその塩による処理の後、残存塩素除去処理を実施してもよい。ここで、残存塩素除去処理とは、次亜塩素酸ナトリウムによる反応を終了させる為に、反応中の澱粉懸濁液に亜硫酸水素ナトリウム、亜硫酸ナトリウム、ピロ亜硫酸ナトリウム、アスコルビン酸ナトリウムなどの還元剤を添加することを意味する。還元剤は固体または溶液のいずれであってもよい。また、還元剤の添加量は、次亜塩素酸の添加量や残留している残存塩素量に応じて適宜調整することができる。 In the production method according to the present invention, the residual chlorine removal treatment may be performed after the treatment with hypochlorous acid or a salt thereof. Here, residual chlorine removal treatment means that a reducing agent such as sodium bisulfite, sodium sulfite, sodium pyrosulfite, or sodium ascorbate is added to the starch suspension during the reaction in order to terminate the reaction with sodium hypochlorite. It means adding. The reducing agent may be either solid or solution. Moreover, the addition amount of a reducing agent can be suitably adjusted according to the addition amount of hypochlorous acid, and the residual chlorine amount which remains.
残存塩素量はKIチェック法により確認することができる。KIチェック法は以下のように実施できる。すなわち、濾紙に1N硫酸を数滴添加し、その上に澱粉懸濁液を数滴添加して馴染ませる。その上に10%ヨウ化カリウム溶液を数滴添加し、変色が認められた場合は塩素が残留していることを意味する。変色が認められなかった場合は塩素が残留しておらず、残存塩素除去処理が完全に行なわれたことを意味する。 The amount of residual chlorine can be confirmed by the KI check method. The KI check method can be implemented as follows. That is, a few drops of 1N sulfuric acid is added to the filter paper, and then a few drops of the starch suspension are added to the filter paper to adjust. When a few drops of 10% potassium iodide solution are added to the solution and discoloration is observed, it means that chlorine remains. When no discoloration was observed, chlorine did not remain, meaning that the residual chlorine removal process was completely performed.
本発明による製造方法では、澱粉を次亜塩素酸またはその塩で処理した後、食品用加工澱粉を得るための加工処理を行う。次亜塩素酸またはその塩で処理した澱粉は、そのまま加工処理に供してもよいし、あるいは、一旦乾燥させた後に水に再懸濁したものを加工処理に供してもよい。 In the production method according to the present invention, starch is treated with hypochlorous acid or a salt thereof, and then processed to obtain a processed starch for food. The starch treated with hypochlorous acid or a salt thereof may be subjected to processing as it is, or may be subjected to processing after being once dried and resuspended in water.
食品用加工澱粉を得るための加工処理としては、一般的には様々なものが知られているが、典型的には澱粉の物性や性質を改変する化学的加工処理が挙げられる。本発明に用いられる加工処理は、pH9.5〜11.5で高い反応率を示す化学的加工処理であり、具体的にはヒドロキシプロピル化処理、リン酸架橋処理、および酢酸ビニルモノマーを用いたアセチル化処理からなる群から選択される。これらの加工処理はそれぞれ単独で行ってもよいし、2種以上の加工処理を組み合わせて行ってもよい。これらの加工処理は、必要な試薬、すなわち、ヒドロキシプロピル化剤、リン酸架橋剤、または酢酸ビニルモノマーを用いて行われる。また、これらの加工処理は、pH9.5〜11.5の条件下で行なうことが好ましい。その他の具体的な条件は、当業者であれば適宜設定することができる。 Various processing is generally known as processing for obtaining processed starch for food, and typically includes chemical processing for modifying the physical properties and properties of starch. The processing used in the present invention is a chemical processing that exhibits a high reaction rate at pH 9.5 to 11.5. Specifically, hydroxypropylation treatment, phosphoric acid crosslinking treatment, and vinyl acetate monomer were used. It is selected from the group consisting of acetylation treatment. Each of these processing treatments may be performed alone or in combination of two or more processing treatments. These processings are performed using the necessary reagents, ie, hydroxypropylating agent, phosphoric acid cross-linking agent, or vinyl acetate monomer. Moreover, these processing treatments are preferably performed under conditions of pH 9.5 to 11.5. Other specific conditions can be appropriately set by those skilled in the art.
本発明では、化学的加工処理を実施した場合には、必要に応じて物理的加工処理を追加して実施してもよい。物理的加工処理としては、α化、湿熱処理、油脂加工、酵素処理、酸処理、アルカリ処理、温水処理、ボールミル処理、高圧処理が挙げられる。 In the present invention, when chemical processing is performed, physical processing may be additionally performed as necessary. Examples of the physical processing treatment include pregelatinization, wet heat treatment, fat and oil processing, enzyme treatment, acid treatment, alkali treatment, hot water treatment, ball mill treatment, and high pressure treatment.
本発明による製造方法により得られた食品用加工澱粉は、和洋菓子類、タレ、ソース、ドレッシング、フィリング、水産・畜産練り食品、麺類など、幅広く食品に用いることができる。また、本発明による製造方法により得られた食品用加工澱粉は、医薬品の製剤用添加剤としても用いることができる。すなわち、本発明において「食品用加工澱粉」とは食品のみならず医薬品における使用態様も含む意味で用いられるものとする。 The processed starch for foods obtained by the production method according to the present invention can be used in a wide variety of foods such as Japanese and Western confectionery, sauces, sauces, dressings, fillings, fishery / livestock pasteurized foods, and noodles. The processed starch for food obtained by the production method according to the present invention can also be used as an additive for pharmaceutical preparations. That is, in the present invention, “processed starch for food” is used in the meaning including not only foods but also usage modes in pharmaceuticals.
本発明による製造方法により得られた食品用加工澱粉は、高い白度を有する。従って、本発明による製造方法は、パン類、コロッケ、メンチカツ、ハンバーグなどの各種惣菜類、食肉加工品、スナック菓子、スープ、飲料、和菓子、洋菓子、タレ・ソース類、麺類、水産・畜産練製品、錠剤、タブレットなどの高い白度が求められる食品や医薬品の製造に用いることができるとともに、漂白処理に用いる薬剤の使用量を低減し、製造コストを低減できる点、有効塩素濃度に由来する塩素臭を低減する点で有利である。 The processed starch for food obtained by the production method according to the present invention has high whiteness. Accordingly, the production method according to the present invention includes various prepared foods such as breads, croquettes, mentaka cuts, hamburgers, processed meat products, snack confectionery, soups, beverages, Japanese confectionery, western confectionery, sauces, sauces, noodles, marine products and livestock products. It can be used in the manufacture of foods and pharmaceuticals that require high whiteness, such as tablets and tablets, and the amount of chemicals used for bleaching can be reduced to reduce manufacturing costs. Chlorine odor derived from effective chlorine concentration This is advantageous in terms of reducing.
以下の例に基づいて本発明を具体的に説明するが、本発明はこれらの例に限定されるものではない。 The present invention will be specifically described based on the following examples, but the present invention is not limited to these examples.
実施例1−1
未処理のタピオカ澱粉(白度80.2)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いでアルカリ剤を添加してpH10に調整した後、酢酸ビニルモノマーを16.5g添加して30分間アセチル化反応を行った。その後、塩酸を添加してpHを酸性に調整することでアセチル化反応を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Example 1-1
Water was added to 300 g of untreated tapioca starch (whiteness 80.2) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Subsequently, after adding an alkali agent and adjusting to pH 10, 16.5g of vinyl acetate monomers were added and acetylation reaction was performed for 30 minutes. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the acetylation reaction. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
次亜塩素酸ナトリウムの有効塩素は以下の方法によって定量される。約10gの次亜塩素酸ナトリウム試料を精秤し、200mlのメスフラスコに移した後、蒸留水を加えて200mlの試料溶液とする。この試料溶液10mlを200ml共栓付き三角フラスコに採り、10%ヨウ化カリウム溶液20mlと30%硫酸20mlを加え、混合する。これを暗所にて5分間静置した後、0.05Nチオ硫酸ナトリウムで無色化するまで滴定する。空試験では、試料溶液に蒸留水10mlを用いて同様の操作を行う。有効塩素は以下の計算式を用いて算出する。 The effective chlorine of sodium hypochlorite is quantified by the following method. About 10 g of sodium hypochlorite sample is precisely weighed and transferred to a 200 ml volumetric flask, and then distilled water is added to make a 200 ml sample solution. Take 10 ml of this sample solution in an Erlenmeyer flask with a 200 ml stopper, add 20 ml of 10% potassium iodide solution and 20 ml of 30% sulfuric acid, and mix. This is left to stand in the dark for 5 minutes, and then titrated with 0.05N sodium thiosulfate until colorless. In the blank test, the same operation is performed using 10 ml of distilled water as the sample solution. Effective chlorine is calculated using the following formula.
また、KIチェックは以下の方法によって行われる有効塩素の簡易検出方法である。濾紙に1N硫酸を数滴添加し、その上に澱粉懸濁液を数滴添加して馴染ませる。その上に10%ヨウ化カリウム溶液を数滴添加し、変色が認められた場合は有効塩素が残留していると判定する。一方、変色が認められなかった場合は有効塩素が残留していないと判定する。 The KI check is a simple detection method of effective chlorine performed by the following method. Add a few drops of 1N sulfuric acid to the filter paper and add a few drops of starch suspension on top of it to acclimate. A few drops of 10% potassium iodide solution is added to the solution, and when discoloration is observed, it is determined that effective chlorine remains. On the other hand, when no discoloration is observed, it is determined that no effective chlorine remains.
実施例1−2
次亜塩素酸ナトリウムの添加量を5.54g(澱粉乾物質量に対する有効塩素として2400ppm)とし、その他の操作を実施例1−1と同様に操作して澱粉試料を得た。
Example 1-2
The amount of sodium hypochlorite added was 5.54 g (2400 ppm as effective chlorine based on the amount of starch dry substance), and other operations were performed in the same manner as in Example 1-1 to obtain starch samples.
実施例1−3
原料澱粉を未処理のワキシーコーンスターチ(白度82.0)とし、その他の操作を実施例1−1と同様に操作して澱粉試料を得た。
Example 1-3
The raw material starch was untreated waxy corn starch (whiteness 82.0), and other operations were performed in the same manner as in Example 1-1 to obtain starch samples.
実施例1−4
未処理のタピオカ澱粉(白度80.2)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いでpH緩衝剤1.5gとアルカリ剤を添加してpH11に調整した後、トリメタリン酸ナトリウムを0.36g添加して60分間リン酸架橋反応を行った。その後、塩酸を添加してpHを酸性に調整することでリン酸架橋反応を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Example 1-4
Water was added to 300 g of untreated tapioca starch (whiteness 80.2) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, 1.5 g of pH buffer and an alkali agent were added to adjust the pH to 11, and then 0.36 g of sodium trimetaphosphate was added to carry out a phosphoric acid crosslinking reaction for 60 minutes. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the phosphoric acid crosslinking reaction. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
実施例1−5
未処理のワキシーコーンスターチ(白度82.0)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いでpH緩衝剤6.0gとアルカリ剤を添加してpH11に調整した後、酸化プロピレンを21.0g添加して18時間ヒドロキシプロピル化反応を行った。その後、塩酸を添加してpHを酸性に調整することでヒドロキシプロピル化反応を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Example 1-5
Water was added to 300 g of untreated waxy corn starch (whiteness 82.0) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Subsequently, 6.0 g of a pH buffer and an alkali agent were added to adjust the pH to 11, and then 21.0 g of propylene oxide was added to carry out a hydroxypropylation reaction for 18 hours. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the hydroxypropylation reaction. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例1−1
次亜塩素酸ナトリウムとピロ亜硫酸ナトリウムの添加及び反応を行わず、その他の操作を実施例1−1と同様に操作して澱粉試料を得た。
Comparative Example 1-1
Addition and reaction of sodium hypochlorite and sodium pyrosulfite were not performed, and other operations were performed in the same manner as in Example 1-1 to obtain starch samples.
比較例1−2
次亜塩素酸ナトリウムとピロ亜硫酸ナトリウムの添加及び反応を行わず、その他の操作を実施例1−3と同様に操作して澱粉試料を得た。
Comparative Example 1-2
Addition and reaction of sodium hypochlorite and sodium pyrosulfite were not performed, and other operations were performed in the same manner as in Example 1-3 to obtain a starch sample.
比較例1−3
次亜塩素酸ナトリウムとピロ亜硫酸ナトリウムの添加及び反応を行わず、その他の操作を実施例1−4と同様に操作して澱粉試料を得た。
Comparative Example 1-3
Addition and reaction of sodium hypochlorite and sodium pyrosulfite were not performed, and other operations were performed in the same manner as in Example 1-4 to obtain starch samples.
比較例1−4
次亜塩素酸ナトリウムとピロ亜硫酸ナトリウムの添加及び反応を行わず、その他の操作を実施例1−5と同様に操作して澱粉試料を得た。
Comparative Example 1-4
Addition and reaction of sodium hypochlorite and sodium pyrosulfite were not performed, and other operations were performed in the same manner as in Example 1-5 to obtain starch samples.
比較例2−1
未処理のタピオカ澱粉(白度80.2)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いでアルカリ剤を添加してpH10に調整した後、酢酸ビニルモノマーを16.5g添加して30分間アセチル化反応を行った。その後、塩酸を添加してpHを酸性に調整することでアセチル化反応を終了した。次いで次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 2-1
Water was added to 300 g of untreated tapioca starch (whiteness 80.2) to prepare a starch suspension having a solid content of 40 (w / w)%. Subsequently, after adding an alkali agent and adjusting to pH 10, 16.5g of vinyl acetate monomers were added and acetylation reaction was performed for 30 minutes. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the acetylation reaction. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added, and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例2−2
次亜塩素酸ナトリウムの添加量を5.54g(澱粉乾物質量に対する有効塩素として2400ppm)とし、その他の操作を比較例2−1と同様に操作して澱粉試料を得た。
Comparative Example 2-2
The amount of sodium hypochlorite added was 5.54 g (2400 ppm as effective chlorine with respect to the amount of dry substance of starch), and other operations were performed in the same manner as in Comparative Example 2-1, to obtain a starch sample.
比較例2−3
未処理のワキシーコーンスターチ(白度82.0)とし、その他の操作を比較例2−1と同様に操作して澱粉試料を得た。
Comparative Example 2-3
An untreated waxy corn starch (whiteness 82.0) was used, and other operations were performed in the same manner as in Comparative Example 2-1, to obtain a starch sample.
比較例2−4
未処理のタピオカ澱粉(白度80.2)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いでpH緩衝剤1.5gとアルカリ剤を添加してpH11に調整した後、トリメタリン酸ナトリウムを0.36g添加して60分間リン酸架橋反応を行った。その後、塩酸を添加してpHを酸性に調整することでリン酸架橋反応を終了した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 2-4
Water was added to 300 g of untreated tapioca starch (whiteness 80.2) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 1.5 g of pH buffer and an alkali agent were added to adjust the pH to 11, and then 0.36 g of sodium trimetaphosphate was added to carry out a phosphoric acid crosslinking reaction for 60 minutes. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the phosphoric acid crosslinking reaction. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例2−5
未処理のワキシーコーンスターチ(白度82.0)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いでpH緩衝剤6.0gとアルカリ剤を添加してpH11に調整した後、酸化プロピレンを21.0g添加して18時間ヒドロキシプロピル化反応を行った。その後、塩酸を添加してpHを酸性に調整することでヒドロキシプロピル化反応を終了した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 2-5
Water was added to 300 g of untreated waxy corn starch (whiteness 82.0) to prepare a starch suspension having a solid content of 40 (w / w)%. Subsequently, 6.0 g of a pH buffer and an alkali agent were added to adjust the pH to 11, and then 21.0 g of propylene oxide was added to carry out a hydroxypropylation reaction for 18 hours. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the hydroxypropylation reaction. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例3−1
未処理のタピオカ澱粉(白度80.2)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いでアルカリ剤を添加してpH8.5に調整した後、無水酢酸24gを180分間かけて添加し、その間にも適宜アルカリ剤を添加してpH8.5を維持してアセチル化反応を行った。その後、塩酸を添加してpHを酸性に調整することでアセチル化反応を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 3-1
Water was added to 300 g of untreated tapioca starch (whiteness 80.2) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, an alkali agent was added to adjust the pH to 8.5, and then 24 g of acetic anhydride was added over 180 minutes, and an alkali agent was appropriately added during that time to maintain pH 8.5 to carry out an acetylation reaction. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the acetylation reaction. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例3−2
未処理のタピオカ澱粉(白度80.2)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いでアルカリ剤を添加してpH8.5に調整した後、無水酢酸24gを180分間かけて添加し、その間にも適宜アルカリ剤を添加してpH8.5を維持してアセチル化反応を行った。その後、塩酸を添加してpHを酸性に調整することでアセチル化反応を終了した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 3-2
Water was added to 300 g of untreated tapioca starch (whiteness 80.2) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, an alkali agent was added to adjust the pH to 8.5, and then 24 g of acetic anhydride was added over 180 minutes, and an alkali agent was appropriately added during that time to maintain pH 8.5 to carry out an acetylation reaction. Thereafter, hydrochloric acid was added to adjust the pH to acidic, thereby terminating the acetylation reaction. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例4−1
未処理のワキシーコーンスターチ(白度82.0)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いでアルカリ剤を添加してpH8.5に調整した後、無水酢酸15gにアジピン酸0.36gを完全に溶解した溶液を120分間かけて添加し、その間にも適宜アルカリ剤を添加してpH8.5を維持してアセチル化アジピン酸架橋反応を行った。その後、塩酸を添加してpHを酸性に調整することでアセチル化アジピン酸架橋反応を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 4-1
Water was added to 300 g of untreated waxy corn starch (whiteness 82.0) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, an alkaline agent was added to adjust the pH to 8.5, and then a solution in which 0.36 g of adipic acid was completely dissolved in 15 g of acetic anhydride was added over 120 minutes. The acetylated adipic acid crosslinking reaction was conducted while maintaining 5. Then, the acetylated adipic acid crosslinking reaction was completed by adjusting the pH to acidic by adding hydrochloric acid. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例4−2
未処理のワキシーコーンスターチ(白度82.0)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いでアルカリ剤を添加してpH8.5に調整した後、無水酢酸15gにアジピン酸0.36gを完全に溶解した溶液を120分間かけて添加し、その間にも適宜アルカリ剤を添加してpH8.5を維持してアセチル化アジピン酸架橋反応を行った。その後、塩酸を添加してpHを酸性に調整することでアセチル化アジピン酸架橋反応を終了した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 4-2
Water was added to 300 g of untreated waxy corn starch (whiteness 82.0) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, an alkaline agent was added to adjust the pH to 8.5, and then a solution in which 0.36 g of adipic acid was completely dissolved in 15 g of acetic anhydride was added over 120 minutes. The acetylated adipic acid crosslinking reaction was conducted while maintaining 5. Then, the acetylated adipic acid crosslinking reaction was completed by adjusting the pH to acidic by adding hydrochloric acid. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例5−1
未処理のワキシーコーンスターチ(白度82.0)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いでアルカリ剤を添加してpH9.0に調整した後、無水オクテニルコハク酸6gを60分間かけて添加し、その間にも適宜アルカリ剤を添加してpH9.0を維持してオクテニルコハク酸反応を行った。その後、塩酸を添加してpHを酸性に調整することでオクテニルコハク酸反応を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 5-1
Water was added to 300 g of untreated waxy corn starch (whiteness 82.0) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, an alkaline agent was added to adjust the pH to 9.0, and then 6 g of octenyl succinic anhydride was added over 60 minutes, and an alkenyl succinic acid reaction was performed while maintaining the pH at 9.0 by appropriately adding an alkaline agent in the meantime. . Then, the octenyl succinic acid reaction was complete | finished by adding hydrochloric acid and adjusting pH to acidity. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
比較例5−2
未処理のワキシーコーンスターチ(白度82.0)300gに水を加え、固形分40(w/w)%の澱粉懸濁液を調製した。次いでアルカリ剤を添加してpH9.0に調整した後、無水オクテニルコハク酸6gを60分間かけて添加し、その間にも適宜アルカリ剤を添加してpH9.0を維持してオクテニルコハク酸反応を行った。その後、塩酸を添加してpHを酸性に調整することでオクテニルコハク酸反応を終了した。次いで、次亜塩素酸ナトリウムを2.77g(澱粉乾物質量に対する有効塩素として1200ppm)添加して30分間漂白処理を行った。その後、KIチェックにおいて澱粉懸濁液から有効塩素が検出されなくなるまでピロ亜硫酸ナトリウムを添加することで漂白処理を終了した。次いで、この澱粉懸濁液を5倍量の水で2回洗浄し、生じた澱粉ケーキを40℃で7時間乾燥して水分15%以下に調整した。これをミキサーで粉砕し、50メッシュを通したものを澱粉試料とした。
Comparative Example 5-2
Water was added to 300 g of untreated waxy corn starch (whiteness 82.0) to prepare a starch suspension having a solid content of 40 (w / w)%. Next, an alkaline agent was added to adjust the pH to 9.0, and then 6 g of octenyl succinic anhydride was added over 60 minutes, and an alkenyl succinic acid reaction was performed while maintaining the pH at 9.0 by appropriately adding an alkaline agent in the meantime. . Then, the octenyl succinic acid reaction was complete | finished by adding hydrochloric acid and adjusting pH to acidity. Next, 2.77 g of sodium hypochlorite (1200 ppm as effective chlorine with respect to the amount of dry substance of starch) was added and bleaching was performed for 30 minutes. Thereafter, the bleaching treatment was completed by adding sodium pyrosulfite until no effective chlorine was detected from the starch suspension in the KI check. Next, this starch suspension was washed twice with 5 times the amount of water, and the resulting starch cake was dried at 40 ° C. for 7 hours to adjust the water content to 15% or less. This was pulverized with a mixer and passed through 50 mesh to obtain a starch sample.
試験例1:白度の測定
測定には色差計SE2000型(日本電色工業株式会社製)を用いる。測定方法を反射に設定し、標準白板SE−15723(X:95.29、Y:93.42、Z:112.80)にて標準合わせを行なう。次いで、澱粉試料が隙間なく充填された直径30mmのガラスセルの色差を5回測定し、5回の測定で得られたWBの平均値を白度とする。
Test Example 1: A color difference meter SE2000 type (manufactured by Nippon Denshoku Industries Co., Ltd.) is used for measurement of whiteness . The measurement method is set to reflection, and standard alignment is performed with a standard white plate SE-15723 (X: 95.29, Y: 93.42, Z: 112.80). Next, the color difference of a glass cell with a diameter of 30 mm filled with a starch sample without gaps is measured five times, and the average value of WB obtained by the five measurements is defined as whiteness.
試験例2:カルボキシル基含量の測定
カルボキシル基含量は、以下の方法によって定量される。乾燥物質量5.0gの澱粉試料に0.1N塩酸50mlを加え、30分間攪拌した後、孔径10〜16μmのガラスフィルターを用いて吸引濾過し、濾液が塩化物の反応を呈さなくなるまで蒸留水で洗浄を続ける。塩化物の反応は、濾液に0.1N硝酸銀溶液を添加することで確認することができ、濾液が白濁すれば塩化物反応が起こっていることとなる。残留物を水300mlに懸濁し、攪拌しながら水浴上で加熱してゲル化させ、さらに15分間加熱した後、フェノールフタレイン指示薬を3滴加え、直ちに0.1N水酸化ナトリウム溶液で呈色するまですばやく滴定する。空試験では、乾燥物質量5.0gの澱粉試料に蒸留水50mlを加え、30分間攪拌した後、孔径10〜16μmのガラスフィルターを用いて吸引濾過し、蒸留水200mlで洗う。残留物を蒸留水300mlに懸濁し、攪拌しながら水浴上で加熱してゲル化させ、さらに15分間加熱した後、フェノールフタレイン指示薬を3滴加え、直ちに0.1N水酸化ナトリウム溶液で呈色するまですばやく滴定する。カルボキシル基含量は以下の計算式を用いて算出する。
Test Example 2: Measurement of carboxyl group content The carboxyl group content is quantified by the following method. After adding 50 ml of 0.1N hydrochloric acid to a starch sample having a dry substance amount of 5.0 g, stirring for 30 minutes, suction filtration is performed using a glass filter having a pore size of 10 to 16 μm, and distilled water is used until the filtrate does not exhibit chloride reaction. Continue cleaning with. Chloride reaction can be confirmed by adding a 0.1N silver nitrate solution to the filtrate. If the filtrate becomes cloudy, a chloride reaction has occurred. The residue is suspended in 300 ml of water, heated on a water bath with stirring to gel, and further heated for 15 minutes, then 3 drops of phenolphthalein indicator are added and immediately colored with 0.1N sodium hydroxide solution. Titration quickly. In the blank test, 50 ml of distilled water is added to a starch sample having a dry substance amount of 5.0 g, stirred for 30 minutes, suction filtered using a glass filter having a pore size of 10 to 16 μm, and washed with 200 ml of distilled water. The residue is suspended in 300 ml of distilled water, heated on a water bath with stirring to gel, and further heated for 15 minutes. Then, 3 drops of phenolphthalein indicator is added and immediately colored with 0.1N sodium hydroxide solution. Titrate quickly until The carboxyl group content is calculated using the following formula.
試験例3:カルボキシル基の確認試験
澱粉試料0.5gを1%メチレンブルー溶液25mlに懸濁し、5〜10分間時々攪拌後、上澄液を傾斜して除き、沈澱を水で十分に洗う。得られた沈殿物の一部を採取し、顕微鏡で観察する。顕微鏡観察において、澱粉粒に暗青色の着色が観察される場合を陽性とし、暗青色の着色が観察されない場合を陰性とする。また、陽性と陰性の区別が困難であると判断した場合は擬陽性とする。
Test Example 3: Confirmation Test for Carboxyl Group 0.5 g of a starch sample is suspended in 25 ml of 1% methylene blue solution, stirred occasionally for 5 to 10 minutes, and then the supernatant is decanted and the precipitate is thoroughly washed with water. Part of the resulting precipitate is collected and observed with a microscope. In microscopic observation, the case where dark blue coloration is observed in starch granules is positive, and the case where dark blue coloration is not observed is negative. In addition, if it is determined that it is difficult to distinguish between positive and negative, a false positive is assumed.
試験例4:アミログラム測定
無水物換算で6%に調製した澱粉スラリーの糊化特性を、アミログラフを用いて測定した(測定条件:30℃で測定を開始した後、1.5℃/分で95℃まで昇温させ、その後95℃を30分間維持した)。アミログラム測定結果から、95℃・0分時の粘度を読み取り、これをアミロ粘度とした。アミロ粘度が低いほどリン酸架橋の架橋度が高い傾向があるため、架橋度の指標とした(アミロ粘度が低いほど架橋度が高い)。
Test Example 4: Measurement of amylogram The gelatinization property of starch slurry prepared to 6% in terms of anhydride was measured using an amylograph (measurement conditions: 95% at 1.5 ° C./min after starting measurement at 30 ° C. The temperature was raised to 0 ° C., and then maintained at 95 ° C. for 30 minutes). From the amylogram measurement result, the viscosity at 95 ° C. and 0 minutes was read, and this was taken as the amylo viscosity. Since the crosslinking degree of phosphoric acid crosslinking tends to be higher as the amylo viscosity is lower, it was used as an index of the crosslinking degree (the lower the amylo viscosity, the higher the crosslinking degree).
試験例1〜4の結果を示すと下記表の通りであった。 The results of Test Examples 1 to 4 are shown in the following table.
上記結果から明らかなように、次亜塩素酸による処理を加工処理の前に実施した場合の白度(実施例1−1〜1−5)は、次亜塩素酸による処理を行わなかった場合の白度(比較例1−1〜1−4)、および次亜塩素酸による処理を加工処理の後に実施した場合の白度(比較例2−1〜2−5)よりも顕著に高かった。また、加工処理として、pH10におけるVAMによるアセチル化、pH11におけるリン酸架橋およびpH11におけるヒドロキシプロピル化を実施した場合の白度(実施例1−1〜1−5)は、pH8.5におけるAAによるアセチル化(比較例3−1および3−2)、pH8.5におけるアセチル化アジピン酸架橋(比較例4−1および4−2)、pH9.0におけるオクテニルコハク酸反応(比較例5−1および5−2)を実施した場合の白度よりも顕著に高かった。さらに、次亜塩素酸による処理の後にリン酸架橋を実施した場合のアミロ粘度(実施例1−4)は、次亜塩素酸による処理を行わずにリン酸架橋を実施した場合のアミロ粘度(比較例1−3)、および次亜塩素酸による処理の前にリン酸架橋を実施した場合のアミロ粘度(比較例2−4)よりも顕著に低かった。よって、リン酸架橋処理の前に次亜塩素酸による処理を実施すると、澱粉粒の膨潤が抑制され、リン酸架橋の反応率(架橋度)が向上することが示された。 As is clear from the above results, the whiteness (Examples 1-1 to 1-5) when the treatment with hypochlorous acid was carried out before the processing was performed when the treatment with hypochlorous acid was not carried out. Whiteness (Comparative Examples 1-1 to 1-4) and whiteness (Comparative Examples 2-1 to 2-5) when the treatment with hypochlorous acid was carried out after the processing was significantly higher . Further, as processing, acetylation with VAM at pH 10, phosphoric acid cross-linking at pH 11 and hydroxypropylation at pH 11 (Examples 1-1 to 1-5) are based on AA at pH 8.5. Acetylation (Comparative Examples 3-1 and 3-2), acetylated adipic acid bridge at pH 8.5 (Comparative Examples 4-1 and 4-2), octenyl succinic acid reaction at pH 9.0 (Comparative Examples 5-1 and 5) -2) was significantly higher than the whiteness in the case of carrying out. Furthermore, the amyloviscosity (Example 1-4) in the case of carrying out phosphoric acid crosslinking after the treatment with hypochlorous acid is the amyloviscosity in the case where phosphoric acid crosslinking is carried out without carrying out the treatment with hypochlorous acid ( It was significantly lower than the comparative example 1-3) and the amylo viscosity (comparative example 2-4) when phosphoric acid crosslinking was carried out before the treatment with hypochlorous acid. Therefore, it was shown that when the treatment with hypochlorous acid was carried out before the phosphoric acid crosslinking treatment, the swelling of the starch granules was suppressed and the reaction rate (crosslinking degree) of phosphoric acid crosslinking was improved.
澱粉に化学的加工処理を施す場合、加工試薬の反応性を高めるために反応系をアルカリ性に調整することが行われることがあるが、アルカリ性に調整することで澱粉が褐色に変化して白度が大きく低下し、その後中和しても澱粉の白度は元に戻らず、白度は低い値を示すことになる。しかしながら、澱粉に高い白度が求められる食品や医薬品においてはこのように白度が低下した澱粉は望ましくなく、好ましくは、白度が90以上、より好ましくは白度が92以上の澱粉を安定的に供給する必要がある。本発明による方法により製造された加工澱粉はこのような高い白度を満たすものであり、本発明による製造方法は、高い白度が求められる食品や医薬品に用いられる加工澱粉の製造に有用である。 When chemical processing is applied to starch, the reaction system may be adjusted to be alkaline in order to increase the reactivity of the processing reagents. However, even after neutralization, the whiteness of the starch does not return to the original value, and the whiteness shows a low value. However, in foods and pharmaceuticals where high whiteness is required for starch, starch with such reduced whiteness is not desirable, and preferably starch with a whiteness of 90 or more, more preferably with a whiteness of 92 or more is stable. Need to supply. The processed starch produced by the method according to the present invention satisfies such high whiteness, and the production method according to the present invention is useful for the production of processed starch used in foods and pharmaceuticals that require high whiteness. .
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