KR20230080006A - Manufacturing method of modified starch with stable viscosity expression and high resistant starch content - Google Patents
Manufacturing method of modified starch with stable viscosity expression and high resistant starch content Download PDFInfo
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- 235000019426 modified starch Nutrition 0.000 title claims abstract description 110
- 239000004368 Modified starch Substances 0.000 title claims abstract description 109
- 229920000294 Resistant starch Polymers 0.000 title claims abstract description 51
- 235000021254 resistant starch Nutrition 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 229920002472 Starch Polymers 0.000 claims abstract description 170
- 235000019698 starch Nutrition 0.000 claims abstract description 169
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 51
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 20
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 20
- 239000001630 malic acid Substances 0.000 claims description 20
- 235000011090 malic acid Nutrition 0.000 claims description 20
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- 230000035484 reaction time Effects 0.000 claims description 8
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- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000546 pharmaceutical excipient Substances 0.000 abstract description 3
- 239000002562 thickening agent Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 description 47
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 23
- 229920002261 Corn starch Polymers 0.000 description 20
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- 239000008213 purified water Substances 0.000 description 17
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- 102000004190 Enzymes Human genes 0.000 description 3
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- 102000004139 alpha-Amylases Human genes 0.000 description 2
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- 239000008280 blood Substances 0.000 description 2
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- ZDGGJQMSELMHLK-UHFFFAOYSA-N m-Trifluoromethylhippuric acid Chemical compound OC(=O)CNC(=O)C1=CC=CC(C(F)(F)F)=C1 ZDGGJQMSELMHLK-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
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- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920001592 potato starch Polymers 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
- 238000004148 unit process Methods 0.000 description 2
- JPSKCQCQZUGWNM-UHFFFAOYSA-N 2,7-Oxepanedione Chemical compound O=C1CCCCC(=O)O1 JPSKCQCQZUGWNM-UHFFFAOYSA-N 0.000 description 1
- 206010009944 Colon cancer Diseases 0.000 description 1
- 208000001333 Colorectal Neoplasms Diseases 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 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
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- 239000002253 acid Substances 0.000 description 1
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- 235000013305 food Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001341 hydroxy propyl starch Substances 0.000 description 1
- 235000013828 hydroxypropyl starch Nutrition 0.000 description 1
- 201000001421 hyperglycemia Diseases 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 244000005700 microbiome Species 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 229940116317 potato starch Drugs 0.000 description 1
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- 235000021391 short chain fatty acids Nutrition 0.000 description 1
- 150000004666 short chain fatty acids Chemical class 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
Abstract
본 발명은 전분 슬러리에 유기산을 0.05M 내지 0.5M의 농도가 되게 첨가하고 15~55℃에서 0.5~24 hr 동안 반응을 진행시킨 후, 염기성 용액을 첨가하고 전분 슬러리의 pH를 5~7로 조정하여 중화된 전분 슬러리를 수득하는는 단계; 상기 중화된 전분 슬러리를 여과, 수세 및 건조하여 수분 함량이 5~15%(w/w)인 유기산 처리 전분을 수득하는 단계; 및 상기 유기산 처리 전분을 밀폐된 용기에 넣고 100~150℃에서 2~20 hr 동안 습열처리하여 최종 변성전분을 수득하는 단계를 포함하는 변성전분방법을 제공한다. 본 발명의 방법으로 제조된 변성전분은 저항전분 함량이 적어도 35% 이상이면서, 호화시 점도가 안정적으로 발현되기 때문에 부형제, 증점제 등 일정 수준의 점도가 요구되는 다양한 분야에서 사용될 수 있다.In the present invention, an organic acid is added to the starch slurry to a concentration of 0.05M to 0.5M, the reaction is performed at 15 to 55 ° C. for 0.5 to 24 hr, and then a basic solution is added and the pH of the starch slurry is adjusted to 5 to 7 to obtain a neutralized starch slurry; filtering, washing, and drying the neutralized starch slurry to obtain organic acid-treated starch having a water content of 5 to 15% (w/w); and putting the organic acid-treated starch in an airtight container and subjecting the starch to a wet heat treatment at 100 to 150° C. for 2 to 20 hr to obtain a final modified starch. Since the modified starch prepared by the method of the present invention has a resistant starch content of at least 35% and stable viscosity when gelatinized, it can be used in various fields requiring a certain level of viscosity, such as an excipient and a thickener.
Description
본 발명은 변성전분 제조방법에 관한 것으로서, 더 상세하게는 점도가 안정적으로 발현되어 점성이 요구되는 다양한 제품에 적용될 수 있고 동시에 저항전분 함량이 높은 변성전분 제조방법에 관한 것이다.The present invention relates to a method for producing modified starch, and more particularly, to a method for producing modified starch having a stable viscosity, which can be applied to various products requiring viscosity, and at the same time having a high content of resistant starch.
전분은 인간의 주요 탄수화물 공급원으로서, 소장에서 소화효소의 작용을 받아 포도당 분자로 분해되고 혈액에 흡수되어 우리 몸의 에너지 공급원으로 사용된다. 일반적으로 전분은 소장에서의 소화 형태에 따라 빠른 소화성 전분(rapidly digestible starch, RDS), 느린 소화성 전분(slowly digestible starch, SDS), 및 저항전분(resistant starch, RS)과 같이 3가지로 분류된다(Englyst et al., Classification and measurement of nutritionally important starch fractions. European Journal of Clinical Nutrition 46:33-50., 1992).Starch is the main source of carbohydrates for humans. It is broken down into glucose molecules under the action of digestive enzymes in the small intestine and absorbed into the blood to be used as a source of energy for the body. In general, starch is classified into three types according to the form of digestion in the small intestine: rapidly digestible starch (RDS), slowly digestible starch (SDS), and resistant starch (RS). Englyst et al., Classification and measurement of nutritionally important starch fractions.European Journal of Clinical Nutrition 46:33-50., 1992).
이중 저항전분(Resistant starch)은 난소화성 전분으로도 불리우며, 그 형태에 따라 크게 4가지 유형으로 나뉘는데, 구체적으로 물리적으로 접근이 불가능한 RS 1형, 생전분 입자로 B형의 결정형을 가지며 알파-아밀라아제(α-amylase)에 내성을 갖는 RS 2형, 노화 과정을 통해 형성된 RS 3형 및 화학적 변성에 의해 효소 저항성을 갖는 RS 4형으로 구성된다. 이상과 같이 4가지 유형을 가지는 저항전분의 생리학적 이점에 관한 많은 연구가 이루어져 왔다. 저항전분은 올리고당 및 식이섬유와 비슷한 생리활성을 가지고, 소장에서는 소화 및 흡수가 되지 않고, 식후 혈당 수치를 천천히 증가시키고, 대장에서 미생물에 의해 단쇄 지방산을 생성시킴으로써, 대장암, 고혈당, 고지혈증 등을 예방하고, 지방의 축적을 억제하는 등의 다양한 효능을 가진다. 상기와 같은 효능을 지니며 식이섬유 공급원인 저항전분은 식품 소재로 유용하게 활용될 수 있다.Resistant starch is also called indigestible starch, and is divided into four types according to its form. Specifically, RS 1 type, which is physically inaccessible, and raw starch particles, which have type B crystalline form and alpha-amylase It consists of RS 2 type, which is resistant to (α-amylase), RS 3 type formed through the aging process, and RS 4 type, which has enzyme resistance due to chemical modification. As described above, many studies have been conducted on the physiological benefits of the four types of resistant starch. Resistant starch has physiological activities similar to those of oligosaccharide and dietary fiber, is not digested and absorbed in the small intestine, slowly increases blood sugar levels after meals, and produces short-chain fatty acids by microorganisms in the large intestine, thereby preventing colorectal cancer, hyperglycemia, and hyperlipidemia. It has various effects such as preventing and inhibiting the accumulation of fat. Resistant starch, which has the above effects and is a source of dietary fiber, can be usefully used as a food material.
화학적 변성에 의해 효소 저항성을 갖는 RS 4형의 저항전분은 다양한 공지의 제조방법에 의해 기술로 제조된다 (Modified starches: Properties and Uses, Ed. Wurzburg, CRC Press, Inc., Florida, 1986). RS 4형의 저항전분의 제조방법으로는 가교 결합 반응(cross-linking reaction), 에스테르화 반응(esterification), 에테르화 반응(eterification), 컨버전(conversion) 등이 있다. 보다 구체적으로 가교 결합 반응에 의한 저항전분으로는 가교 결합제, 예를 들어 소듐트리메타포스페이트(STMP), 포스포릴클로아이드, 무수아디핀산 등에 의해 변형된 전분 등이 있고, 에스테르화 반응에 의한 저항전분으로는 인산화 전분, 아세틸화 전분, 옥테닐숙신산 치환 전분 등이 있으며, 에테르화 반응에 의한 저항전분으로는 히드록시프로필 전분 등이 있다. 또한 컨버전 변형에 의한 저항전분으로는 산가수분해 전분, 차아염소산나트륨에 의해 산화된 전분, 효소에 의해 변형된 전분 등이 있다. 상기의 제조방법은 단독으로, 또는 서로 조합되어 사용될 수 있다.Resistant starch of type RS 4, which has enzyme resistance by chemical modification, is manufactured using various known manufacturing methods (Modified starches: Properties and Uses, Ed. Wurzburg, CRC Press, Inc., Florida, 1986). Methods for producing resistant starch of RS 4 type include cross-linking reaction, esterification reaction, etherification reaction, conversion, and the like. More specifically, resistant starch by cross-linking reaction includes starch modified with a cross-linking agent such as sodium trimetaphosphate (STMP), phosphoryl chloride, adipic acid anhydride, etc., and resistant starch by esterification reaction. Examples include phosphorylated starch, acetylated starch, and octenylsuccinic acid-substituted starch, and resistant starch obtained through etherification includes hydroxypropyl starch. In addition, resistant starch by conversion modification includes acid hydrolyzed starch, starch oxidized by sodium hypochlorite, starch modified by enzymes, and the like. The above production methods may be used alone or in combination with each other.
한편, 화학적 가교결합 반응에 의해 제조된 저항전분은 안전성에 대한 의구심이 지속적으로 제기되어 오고 있고, 이를 해결하기 위해 산처리 및 열처리를 병행하여 저항전분의 제조방법이 보고된 바 있다. 예를 들어, 대한민국 공개특허공보 제10-2020-0134765호에는 2~4M 농도의 사과산 용액에 전분을 첨가하는 단계 (a); 상기 단계 (a) 후, 10~20시간 동안 실온 방치하는 단계 (b); 상기 단계 (b) 후, 40~60℃에서 20~30시간 건조하는 단계 (c); 및, 상기 단계 (c) 후, 90~150℃에서 2~12시간 가교반응시키는 단계 (d); 를 포함하는 것을 특징으로 하는 사과산 가교화 전분의 제조방법이 개시되어 있다.On the other hand, doubts about the safety of resistant starch prepared by chemical crosslinking have been continuously raised, and to solve this problem, a method for producing resistant starch using acid treatment and heat treatment in parallel has been reported. For example, Korean Patent Laid-open Publication No. 10-2020-0134765 includes adding starch to a malic acid solution at a concentration of 2 to 4M (a); After step (a), leaving room temperature for 10 to 20 hours (b); Step (c) of drying at 40 to 60° C. for 20 to 30 hours after step (b); And, step (d) of crosslinking reaction at 90 to 150 ° C for 2 to 12 hours after step (c); Disclosed is a method for producing a malic acid crosslinked starch comprising a.
본 발명은 종래의 기술적 배경하에서 도출된 것으로서, 본 발명의 목적은 점도가 안정적으로 발현되고 저항전분 함량이 높은 변성전분의 제조방법을 제공하는데에 있다.The present invention was derived under the conventional technical background, and an object of the present invention is to provide a method for producing modified starch having a stable viscosity and high resistant starch content.
본 발명의 발명자들은 대한민국 공개특허공보 제10-2020-0134765호에 개시된 제조방법으로 제조된 가교화 전분은 저항전분 함량은 높으나 제조 과정 중에 고농도의 사과산을 전분에 고온 조건에서 장시간 처리하기 때문에 전분의 입자 구조가 파괴되고 그로 인해 호화액의 점도가 거의 발현되지 않아 부형제, 증점제 등 일정 수준의 점도가 요구되는 분야에 사용이 어렵다는 점을 확인하고, 이를 해결하기 위해 다양한 단위공정의 조합 또는 공정조건의 조합을 시도하여 변성전분을 제조하였고, 그 결과 소정 이상의 저항전분 함량을 가지면도 동시에 점도가 안정적으로 발현되는 단위공정의 조합 및 공정조건을 확인하고 본 발명을 완성하였다.The inventors of the present invention found that the cross-linked starch prepared by the manufacturing method disclosed in Korean Patent Laid-Open Publication No. 10-2020-0134765 has a high resistant starch content, but during the manufacturing process, high concentration of malic acid is treated with starch under high temperature conditions for a long time, so that the starch It was confirmed that the particle structure is destroyed and, as a result, the viscosity of the gelatinization liquid is hardly expressed, making it difficult to use in areas requiring a certain level of viscosity such as excipients and thickeners. To solve this problem, a combination of various unit processes or process conditions Modified starch was prepared by attempting the combination, and as a result, the present invention was completed by confirming the combination of unit processes and process conditions in which the viscosity is stably expressed even though the resistant starch content is higher than a predetermined level.
상기 목적을 달성하기 위하여, 본 발명은 전분 슬러리에 유기산을 0.05M 내지 0.5M의 농도가 되게 첨가하고 15~55℃에서 0.5~24 hr 동안 반응을 진행시킨 후, 염기성 용액을 첨가하고 전분 슬러리의 pH를 5~7로 조정하여 중화된 전분 슬러리를 수득하는는 단계; 상기 중화된 전분 슬러리를 여과, 수세 및 건조하여 수분 함량이 5~15%(w/w)인 유기산 처리 전분을 수득하는 단계; 및 상기 유기산 처리 전분을 밀폐된 용기에 넣고 100~150℃에서 2~20 hr 동안 습열처리하여 최종 변성전분을 수득하는 단계를 포함하는 변성전분방법을 제공한다.In order to achieve the above object, the present invention adds an organic acid to the starch slurry to a concentration of 0.05M to 0.5M, proceeds with the reaction at 15 to 55 ° C. for 0.5 to 24 hr, and then adds a basic solution to the starch slurry. adjusting the pH to 5-7 to obtain a neutralized starch slurry; filtering, washing, and drying the neutralized starch slurry to obtain organic acid-treated starch having a water content of 5 to 15% (w/w); and putting the organic acid-treated starch in an airtight container and subjecting the starch to a wet heat treatment at 100 to 150° C. for 2 to 20 hr to obtain a final modified starch.
본 발명의 방법으로 제조된 변성전분은 저항전분 함량이 적어도 35% 이상이면서, 호화시 점도가 안정적으로 발현되기 때문에 부형제, 증점제 등 일정 수준의 점도가 요구되는 다양한 분야에서 사용될 수 있다.Since the modified starch prepared by the method of the present invention has a resistant starch content of at least 35% and stable viscosity when gelatinized, it can be used in various fields requiring a certain level of viscosity, such as an excipient and a thickener.
도 1은 본 발명의 제조예 2, 제조예 4, 제조예 7, 비교제조예 2, 비교제조예 4 및 비교제조예 7의 변성전분 제조방법 공정조건과, 단위공정 단계별 pH 변화를 개략적으로 나타낸 것이다.1 schematically shows the process conditions of the modified starch manufacturing method of Preparation Example 2, Preparation Example 4, Preparation Example 7, Comparative Preparation Example 2, Comparative Preparation Example 4, and Comparative Preparation Example 7 of the present invention, and pH change at each unit step. will be.
이하, 본 발명을 구체적으로 설명한다.Hereinafter, the present invention will be described in detail.
본 발명은 점도가 안정적으로 발현되고 저항전분 함량이 높은 변성전분의 제조방법에 관한 것이다.The present invention relates to a method for producing modified starch having a stable viscosity and a high resistant starch content.
본 발명에 따른 변성전분 제조방법은 (a) 전분 슬러리에 유기산을 0.05M 내지 0.5M의 농도가 되게 첨가하고 15~55℃에서 0.5~24 hr 동안 반응을 진행시킨 후, 염기성 용액을 첨가하고 전분 슬러리의 pH를 5~7로 조정하여 중화된 전분 슬러리를 수득하는는 단계; (b) 상기 중화된 전분 슬러리를 여과, 수세 및 건조하여 수분 함량이 5~15%(w/w)인 유기산 처리 전분을 수득하는 단계; 및 (c) 상기 유기산 처리 전분을 밀폐된 용기에 넣고 100~150℃에서 2~20 hr 동안 습열처리하여 최종 변성전분을 수득하는 단계를 포함한다. 이하, 본 발명에 따른 변성전분 제조방법을 각 단계별로 나누어 설명한다.In the method for preparing modified starch according to the present invention, (a) an organic acid is added to a starch slurry at a concentration of 0.05M to 0.5M, the reaction is performed at 15 to 55 ° C. for 0.5 to 24 hr, a basic solution is added, and starch adjusting the pH of the slurry to 5-7 to obtain a neutralized starch slurry; (b) filtering, washing, and drying the neutralized starch slurry to obtain organic acid-treated starch having a water content of 5 to 15% (w/w); and (c) putting the organic acid-treated starch in an airtight container and subjecting the starch to a wet heat treatment at 100 to 150° C. for 2 to 20 hr to obtain final modified starch. Hereinafter, the method for producing modified starch according to the present invention will be described in each step.
(a) 중화된 전분 슬러리를 수득하는는 단계(a) obtaining a neutralized starch slurry
상기 (a) 단계에서 전분 슬러리는 전분을 물(water)에 현탁시킨 것으로서, 전분 슬러리 내에서 전분 농도는 원활한 교반 등을 고려할 때 전분 건조중량을 기준으로 20~40 중량%인 것이 바람직하고, 25~35 중량%인 것이 더 바람직하다. 또한, 상기 전분 슬러리를 구성하는 전분은 변성전분과 대조되는 비변성 전분인 것이 바람직하다. 상기 비변성 전분은 별도의 화학적 또는 생물학적 처리 없이 통상적인 건식제분 또는 습식제분(wet milling) 과정에 의해 생산된 전분을 말한다. 상기 비변성 전분은 옥수수 전분, 찰옥수수 전분, 타피오카 전분, 감자 전분, 고구마 전분, 쌀 전분 또는 밀 전분에서 선택되는 1종 이상일 수 있고, 반응 효율, 안정적인 점도 발현, 저항전분 함량 등을 고려할 때 옥수수 전분인 것이 바람직하다.In the step (a), the starch slurry is a suspension of starch in water, and the starch concentration in the starch slurry is preferably 20 to 40% by weight based on the dry weight of starch in consideration of smooth stirring. more preferably ~35% by weight. In addition, the starch constituting the starch slurry is preferably unmodified starch as opposed to modified starch. The unmodified starch refers to starch produced by a conventional dry milling or wet milling process without separate chemical or biological treatment. The unmodified starch may be one or more selected from corn starch, waxy corn starch, tapioca starch, potato starch, sweet potato starch, rice starch, or wheat starch, and considering reaction efficiency, stable viscosity expression, and resistant starch content, corn It is preferably starch.
상기 (a) 단계에서 유기산은 습식 공정에서 전분과 반응하여 전분의 입자 구조는 거의 파괴하지 않고 전분의 저항전분 함량을 높이는 것이라면 그 종류가 크게 제한되지 않으며, 반응 효율 내지 안전성 등을 고려할 때 아세트산, 젖산, 구연산 또는 사과산에서 선택되는 1종 이상인 것이 바람직하고, 초산, 구연산 또는 사과산에서 선택되는 1종 이상인 것이 더 바람직하다. 또한, 상기 유기산은 후술하는 유기산 처리 전분의 저항전분 함량 내지 점도 등을 고려할 때 전분 슬러리에 0.08M 내지 0.4M의 농도가 되게 첨가되는 것이 바람직하고, 전분 슬러리에 0.1M 내지 0.3M의 농도가 되게 첨가되는 것이 더 바람직하다. 또한, 상기 (a) 단계에서 유기산 첨가 후의 반응 온도는 반응 효율, 후술하는 유기산 처리 전분의 저항전분 함량 내지 점도 등을 고려할 때 18~30℃인 것이 바람직하고 20~25℃인 것이 더 바람직하다. 또한, 유기산 첨가 후의 반응 시간은 후술하는 유기산 처리 전분의 저항전분 함량 내지 점도, 반응 공정의 경제성 등을 고려할 때 1~5 hr인 것이 바람직하고 1~3 hr 인 것이 더 바람직하다.In the step (a), the organic acid reacts with the starch in the wet process, so that the particle structure of the starch is hardly destroyed and the resistant starch content of the starch is increased. It is preferably at least one selected from lactic acid, citric acid, and malic acid, and more preferably at least one selected from acetic acid, citric acid, and malic acid. In addition, the organic acid is preferably added to the starch slurry at a concentration of 0.08M to 0.4M, and the concentration of the organic acid is 0.1M to 0.3M in the starch slurry in consideration of the resistance starch content and viscosity of the organic acid-treated starch, which will be described later. It is more preferable to add In addition, the reaction temperature after adding the organic acid in the step (a) is preferably 18 to 30 ° C., and more preferably 20 to 25 ° C., in consideration of the reaction efficiency and the content or viscosity of resistant starch of the organic acid-treated starch described later. In addition, the reaction time after adding the organic acid is preferably 1 to 5 hr, and more preferably 1 to 3 hr, considering the content or viscosity of resistant starch of the organic acid-treated starch and the economics of the reaction process, which will be described later.
상기 (a) 단계에서 전분과 유기산 간의 반응이 완료된 후 전분 슬러리의 pH를 조정하기 위해 첨가되는 염기성 용액은 수산화나트륨 용액, 수산화칼륨 용액 등 공지의 다양한 염기성 용액에서 선택될 수 있다. 또한, 전분과 유기산 간의 반응이 완료된 후 전분 슬러리의 pH는 후술하는 최종 변성전분의 저항전분 함량 내지 점도 등을 고려할 때 바람직하게는 5~6.5로 조정되고, 더 바람직하게는 5~6의 pH로 조정된다.After completion of the reaction between starch and organic acid in step (a), the basic solution added to adjust the pH of the starch slurry may be selected from various known basic solutions such as sodium hydroxide solution and potassium hydroxide solution. In addition, after completion of the reaction between starch and organic acid, the pH of the starch slurry is preferably adjusted to 5 to 6.5, more preferably to a pH of 5 to 6, considering the content or viscosity of the resistant starch of the final modified starch, which will be described later. Adjusted.
(b) 유기산 처리 전분을 수득하는 단계(b) obtaining organic acid-treated starch
상기 (b) 단계에서 중화된 전분 슬러리는 여과포 등에 의해 여과되고, 여과 과정에서 전분 건조중량 대비 약 5~20배의 물로 수세된다. 수세 후 얻은 케이크 형태의 유기산 처리 전분은 이후 건조 등의 과정을 거쳐 수분 함량이 조정된 고상 형태로 제조된다. 또한, 상기 유기산 처리 전분은 바람직하게는 건조 후 분쇄 과정을 거쳐 분말 형태로 제조될 수 있다. 상기 건조 과정을 거쳐 수득한 유기산 처리 전분의 수분 함량은 후술하는 습열처리 과정의 원활함 등을 고려할 때 6~14%(w/w)인 것이 바람직하고 7~12%(w/w)인 것이 더 바람직하다. 또한, 상기 건조 과정을 거쳐 수득한 유기산 처리 전분은 저항전분 함량이 30~50%이고, 바람직하게는 35~50%이다. 또한, 상기 건조 과정을 거쳐 수득한 유기산 처리 전분은 8 중량% 농도의 호화액 점도가 1400~2000 센티포이즈(Centipoise, cPs)이고 바람직하게는 1450~1900 센티포이즈(Centipoise, cPs)이다.The starch slurry neutralized in the step (b) is filtered with a filter cloth or the like, and washed with water in an amount of about 5 to 20 times the dry weight of the starch during the filtration process. The organic acid-treated starch in the form of a cake obtained after washing with water is then prepared in a solid form in which the moisture content is adjusted through a process such as drying. In addition, the organic acid-treated starch may be preferably prepared in a powder form through a grinding process after drying. The moisture content of the organic acid-treated starch obtained through the drying process is preferably 6 to 14% (w/w), and 7 to 12% (w/w), considering the smoothness of the wet heat treatment process described later. more preferable In addition, the organic acid-treated starch obtained through the drying process has a resistance starch content of 30 to 50%, preferably 35 to 50%. In addition, the organic acid-treated starch obtained through the drying process has a viscosity of 1400 to 2000 centipoise (Centipoise, cPs) and preferably 1450 to 1900 centipoise (Centipoise, cPs) at an 8 wt% concentration.
(c) 최종 변성전분을 수득하는 단계(c) obtaining final modified starch
상기 (c) 단계에서 유기산 처리 전분은 밀폐된 용기에 넣어지고 오토클레이브(Autoclave)와 같은 가열 장치에 옮겨진 후 소정의 고온에서 소정 시간 동안 습열처리된다. 상기 습열처리(Heat Moisture Treatment, HMT)는 오토클레이브와 같은 가열 장치에 의해 가해지는 열과 유기산 처리 전분 내에 존재하는 수분에 의해 전분을 처리하여 전분의 구조를 변경시키는 처리 방법을 말한다. 습열처리 과정에서 전분의 수분 함량이 높으면 호화되기 쉽기 때문에 전분의 수분 함량은 습열처리 전에 바람직하게는 14%(w/w) 이하, 더 바람직하게는 12%(w/w) 이하로 조절된다. 상기 습열처리 온도는 최종 변성전분의 저항전분 함량 내지 점도 등을 고려할 때 110~140℃인 것이 바람직하다. 또한, 습열처리 시간은 최종 변성전분의 저항전분 함량 내지 점도, 경제성 등을 고려할 때 3~15 hr인 것이 바람직하고 5~10 hr 인 것이 더 바람직하다. 상기 습열처리 과정을 거쳐 수득한 최종 변성 전분은 저항전분 함량이 35~55%이고, 바람직하게는 40~55%이다. 또한, 상기 습열처리 과정을 거쳐 수득한 최종 변성전분은 8 중량% 농도의 호화액 점도가 1300~1900 센티포이즈(Centipoise, cPs)이고 바람직하게는 1350~1850 센티포이즈(Centipoise, cPs)이다.In step (c), the organic acid-treated starch is placed in a sealed container, transferred to a heating device such as an autoclave, and subjected to wet heat treatment at a predetermined high temperature for a predetermined time. The heat moisture treatment (HMT) refers to a treatment method of changing the structure of starch by treating starch with heat applied by a heating device such as an autoclave and moisture present in organic acid-treated starch. In the wet heat treatment process, if the moisture content of the starch is high, it is easy to gelatinize, so the moisture content of the starch is preferably adjusted to 14% (w / w) or less, more preferably 12% (w / w) or less before the wet heat treatment. The wet heat treatment temperature is preferably 110 to 140° C. in consideration of the resistance starch content or viscosity of the final modified starch. In addition, the wet heat treatment time is preferably 3 to 15 hr, more preferably 5 to 10 hr, considering the content of resistant starch, viscosity, and economic feasibility of the final modified starch. The final modified starch obtained through the wet heat treatment process has a resistance starch content of 35 to 55%, preferably 40 to 55%. In addition, the final modified starch obtained through the wet heat treatment process has a viscosity of 1300 to 1900 centipoise (Centipoise, cPs), preferably 1350 to 1850 centipoise (Centipoise, cPs), at a concentration of 8% by weight.
이하, 본 발명을 실시예를 통하여 보다 구체적으로 설명한다. 다만 하기 실시예는 본 발명의 기술적 특징을 명확하게 예시하기 위한 것일 뿐, 본 발명의 보호범위를 제한하는 것은 아니다.Hereinafter, the present invention will be described in more detail through examples. However, the following examples are only for clearly illustrating the technical features of the present invention, but do not limit the protection scope of the present invention.
1. 측정방법1. Measurement method
(1) 저항전분 함량(1) Resistant starch content
전분 시료의 저항전분 함량은 Englyst method(Measurement of resistant satarch in vitro and in vivo, 1996)를 이용하여 측정하였다. Englyst method는 사람의 소화 환경을 모사한 in-vitro 시험 방법으로서, 전분 시료에 혼합 소화 효소를 첨가하고 분해한 후, 분해에 의해 생성된 포도당의 양을 GOD-POD 발색 시약으로 정량하고 하기의 수식으로 저항전분 함량을 계산한다.Resistant starch content of starch samples was measured using Englyst method (Measurement of resistant satarch in vitro and in vivo, 1996). Englyst method is an in-vitro test method that simulates the human digestive environment. After adding mixed digestive enzymes to a starch sample and degrading it, the amount of glucose produced by decomposition is quantified with GOD-POD color development reagent, and the following formula is used. Calculate the resistant starch content as
* G : 측정된 포도당 양* G: Measured amount of glucose
* DM : 전분 시료 건조중량* DM: dry weight of starch sample
* RDS(rapidly digestible starch) : 혼합 소화 효소 첨가 후 20분이 경과되었을 때 측정한 소화가능한 전분(DS) 함량(%)으로서 빠른 소화성 전분 함량을 의미함* RDS (rapidly digestible starch): Digestible starch (DS) content (%) measured 20 minutes after the addition of mixed digestive enzymes, which means the content of rapidly digestible starch
* SDS(slowly digestible starch) : 혼합 소화 효소 첨가 후 120분이 경과되었을 때 측정한 소화가능한 전분(DS) 함량(%)으로서 느린 소화성 전분 함량을 의미함* SDS (slowly digestible starch): Digestible starch (DS) content (%) measured 120 minutes after the addition of mixed digestive enzymes, which means the content of slowly digestible starch
(2) 점도(2) Viscosity
전분 시료를 증류수에 현탁하여 전분 시료 농도가 8%(w/w)인 전분 시료 슬러리를 제조하고, RVA 분석기기(모델명 : RVA4500; 공급사 : Perten사)를 이용하여 전분 시료 슬러리를 소정의 온도 프로파일 조건으로 가열 및 냉각시킨 후, 온도 프로파일 조건 중 맨 마지막에 위치하는 13분 경과시의 50℃ 온도에서 최종 점도(Final viscosity)를 측정하였다. RVA 분석을 위한 온도 프로파일 조건은 다음과 같다.The starch sample was suspended in distilled water to prepare a starch sample slurry having a starch sample concentration of 8% (w/w), and the starch sample slurry was subjected to a predetermined temperature profile using an RVA analyzer (model name: RVA4500; supplier: Perten). After heating and cooling under the condition, the final viscosity was measured at 50 ° C. at the end of the temperature profile condition after 13 minutes. The temperature profile conditions for RVA analysis are as follows.
* 0분(50℃); 1분(50℃); 4분 42초(95℃); 7분 12초(95℃); 11분(50℃); 13분(50℃)* 0 min (50° C.); 1 minute (50° C.); 4 min 42 sec (95° C.); 7 min 12 sec (95° C.); 11 minutes (50° C.); 13 minutes (50℃)
2. 유기산 처리 전분의 제조 및 물성 확인2. Preparation of organic acid-treated starch and confirmation of physical properties
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 유기산을 소정의 농도가 되게 첨가하고 혼합한 후 소정의 온도에서 소정의 시간동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 유기산 처리 전분을 수득하였다. 수득한 유기산 처리 전분의 저항전분(RS) 함량(%) 및 점도(8 중량% 농도 전분 시료 슬러리, cPs)를 측정하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, an organic acid was added to the starch slurry to a predetermined concentration, mixed, and reacted at a predetermined temperature for a predetermined time, and then neutralized by adjusting the pH of the starch slurry to about 5.3 ± 0.1 by adding sodium hydroxide solution. made it Filtering and washing with water were performed while adding about 5 times as much purified water to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch. Resistant starch (RS) content (%) and viscosity (8% by weight starch sample slurry, cPs) of the obtained organic acid-treated starch were measured.
하기 표 1 내지 표 4에 유기산 종류, 유기산 처리 농도, 반응 온도, 반응 시간에 따른 유기산 처리 전분의 RS 함량(%) 및 점도(cPs)를 정리하였다. 참고로 상기 유기산 처리 전분을 제조하기 위해 원료료 사용한 옥수수 전분은 저항전분 함량이 약 23.9%이고, 50℃에서 8 중량% 농도의 호화액 점도가 약 1,668 센티포이즈(Centipoise, cPs)이다.In Tables 1 to 4 below, RS content (%) and viscosity (cPs) of organic acid-treated starch according to organic acid type, organic acid treatment concentration, reaction temperature, and reaction time are summarized. For reference, corn starch used as a raw material to prepare the organic acid-treated starch has a resistant starch content of about 23.9%, and a gelatinization viscosity of 8% by weight at 50 ° C. is about 1,668 centipoise (cPs).
상기 표 1 내지 표 4에서 보이는 바와 같이 유기산 처리 전분 제조시 사용한 유기산의 종류에 따른 유기산 처리 전분의 점도 차이는 크지 않은 것으로 나타났다. 한편, 유기산 처리 전분의 저항전분 함량은 유기산으로 아세트산, 구연산 또는 사과산을 사용하고, 유기산의 처리 농도가 0.1M 내지 0.2M이고, 반응 시간이 1.5 hr 전후이고, 반응 온도가 20~25℃인 경우 높은 값을 나타내었다.As shown in Tables 1 to 4, the difference in viscosity of the organic acid-treated starch according to the type of organic acid used in preparing the organic acid-treated starch was not large. On the other hand, the resistant starch content of the organic acid-treated starch is obtained when acetic acid, citric acid, or malic acid is used as the organic acid, the treatment concentration of the organic acid is 0.1 M to 0.2 M, the reaction time is around 1.5 hr, and the reaction temperature is 20-25 ° C. showed high values.
3. 유기산 처리 및 습열처리(Heat Moisture Treatment, HMT)의 조합에 의한 변성전분의 제조 및 물성 확인3. Preparation of modified starch by combination of organic acid treatment and heat moisture treatment (HMT) and confirmation of physical properties
제조예 1.Preparation Example 1.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 아세트산(acetic acid)을 0.1M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.69%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, acetic acid was added to the starch slurry to a concentration of 0.1 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. Filtering and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.69% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 2.Preparation Example 2.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 아세트산(acetic acid)을 0.2M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 11.96%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, acetic acid was added to the starch slurry to a concentration of 0.2M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. Filtering and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 11.96% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 3.Preparation Example 3.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 구연산(citric acid)을 0.1M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.67%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, citric acid was added to the starch slurry to a concentration of 0.1 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. Filtering and washing were performed while adding about 5 times the amount of purified water compared to the dry weight of starch to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.67% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 4.Preparation Example 4.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 구연산(citric acid)을 0.2M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 10.94%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, citric acid was added to the starch slurry to a concentration of 0.2 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. The neutralized starch slurry was filtered and washed while adding about 5 times the amount of purified water compared to the dry weight of the starch, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 10.94% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 5.Preparation Example 5.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 구연산(citric acid)을 0.4M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.05%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, citric acid was added to the starch slurry to a concentration of 0.4 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. Filtering and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.05% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 6.Preparation Example 6.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 사과산(malic acid)을 0.1M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.67%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, malic acid was added to the starch slurry to a concentration of 0.1 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. Filtering and washing were performed while adding about 5 times the amount of purified water compared to the dry weight of starch to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.67% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 7.Preparation Example 7.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 사과산(malic acid)을 0.2M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 10.94%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, malic acid was added to the starch slurry to a concentration of 0.2 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. The neutralized starch slurry was filtered and washed while adding about 5 times the amount of purified water compared to the dry weight of the starch, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 10.94% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
제조예 8.Preparation Example 8.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 사과산(malic acid)을 0.4M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시킨 후, 수산화나트륨 용액을 첨가하여 전분 슬러리의 pH를 약 5.3±0.1로 조정하여 중화시켰다. 중화된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.05%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, malic acid was added to the starch slurry to a concentration of 0.4 M, mixed, and reacted at room temperature (about 20 ° C.) for 90 minutes. Then, sodium hydroxide solution was added to adjust the pH of the starch slurry to about 5.3. Neutralized by adjusting ±0.1. Filtering and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the neutralized starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.05% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 1.Comparative Preparation Example 1.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 아세트산(acetic acid)을 0.1M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 8.21%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, acetic acid was added to the starch slurry to a concentration of 0.1 M, mixed, and the reaction was performed at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the dry weight of the starch to the starch slurry after the reaction, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 8.21% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 2.Comparative Preparation Example 2.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 아세트산(acetic acid)을 0.2M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 10.47%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, acetic acid was added to the starch slurry to a concentration of 0.2M, mixed, and the reaction was performed at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the dry weight of the starch to the starch slurry after the reaction, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 10.47% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 3.Comparative Preparation Example 3.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 구연산(citric acid)을 0.1M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 8.24%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, citric acid was added to the starch slurry to a concentration of 0.1 M, mixed, and then reacted at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding purified water about 5 times the dry weight of starch to the starch slurry after the reaction, and the filter cake was dried to obtain organic acid-treated starch having a water content of about 8.24% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 4.Comparative Preparation Example 4.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 구연산(citric acid)을 0.2M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.89%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, citric acid was added to the starch slurry to a concentration of 0.2M, mixed, and then reacted at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the starch dry weight to the reacted starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.89% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 5.Comparative Preparation Example 5.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 구연산(citric acid)을 0.4M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.56%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, citric acid was added to the starch slurry to a concentration of 0.4M, mixed, and then reacted at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the starch slurry after the reaction, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.56% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 6.Comparative Preparation Example 6.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 사과산(malic acid)을 0.1M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 9.29%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, malic acid was added to the starch slurry to a concentration of 0.1 M, mixed, and then reacted at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the starch dry weight to the reacted starch slurry, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 9.29% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 7.Comparative Preparation Example 7.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 사과산(malic acid)을 0.2M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 9.28%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, malic acid was added to the starch slurry to a concentration of 0.2M, mixed, and then reacted at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the starch slurry after the reaction, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 9.28% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
비교제조예 8.Comparative Preparation Example 8.
옥수수 전분을 증류수에 현탁하여 30%(w/w) 농도의 전분 슬러리를 제조하였다. 이후, 전분 슬러리에 사과산(malic acid)을 0.4M 농도가 되게 첨가하고 혼합한 후 상온(약 20℃)에서 90분 동안 반응을 진행시켰다. 이후 반응이 완료된 전분 슬러리에 전분 건조중량 대비 약 5배수의 정제수를 가하면서 여과 및 수세를 진행하고, 여과 케이크를 건조하여 수분 함량이 약 7.78%(w/w)인 유기산 처리 전분을 수득하였다. 이후, 유기산 처리 전분을 밀폐 용기에 넣고 오토클레이브(Autoclave)로 옮긴 후 약 130℃에서 약 7 hr 동안 습열처리(Heat Moisture Treatment, HMT)하여 최종 변성전분을 수득하였다.Corn starch was suspended in distilled water to prepare a starch slurry with a concentration of 30% (w/w). Thereafter, malic acid was added to the starch slurry to a concentration of 0.4M, mixed, and then reacted at room temperature (about 20° C.) for 90 minutes. Thereafter, filtration and washing were performed while adding about 5 times the purified water compared to the dry weight of starch to the starch slurry after the reaction, and the filter cake was dried to obtain organic acid-treated starch having a moisture content of about 7.78% (w/w). Thereafter, the organic acid-treated starch was placed in an airtight container, transferred to an autoclave, and subjected to heat moisture treatment (HMT) at about 130° C. for about 7 hr to obtain final modified starch.
도 1은 본 발명의 제조예 2, 제조예 4, 제조예 7, 비교제조예 2, 비교제조예 4 및 비교제조예 7의 변성전분 제조방법 공정조건과, 단위공정 단계별 pH 변화를 개략적으로 나타낸 것이다. 또한, 하기 표 5에 제조예 1 내지 제조예 8 및 비교제조예 1 내지 비교제조예 8에서 수득한 변성전분의 저항전분(RS) 함량(%) 및 점도(8 중량% 농도 전분 시료 슬러리, cPs)를 측정하였고, 그 결과를 하기 표 5에 요약하였다.1 schematically shows the process conditions of the modified starch manufacturing method of Preparation Example 2, Preparation Example 4, Preparation Example 7, Comparative Preparation Example 2, Comparative Preparation Example 4, and Comparative Preparation Example 7 of the present invention, and pH change at each unit step. will be. In addition, resistant starch (RS) content (%) and viscosity (8 wt% concentration starch sample slurry, cPs of modified starch obtained in Preparation Examples 1 to 8 and Comparative Preparation Examples 1 to 8 in Table 5 below ) was measured, and the results are summarized in Table 5 below.
상기 표 5에서 보이는 바와 같이 최종 변성전분의 저항전분 함량을 고려할 때 유기산 처리 농도는 0.1M 내지 0.2M이 바람직하였고, 최종 변성전분 호화액의 안정적인 점도 발현을 고려할 때 유기산 처리 후 전분 슬러리의 pH를 약 5~7로 중화한 후 수세 및 여과를 진행하는 것이 필요한 것으로 나타났다. As shown in Table 5, when considering the resistance starch content of the final modified starch, the organic acid treatment concentration was preferably 0.1 M to 0.2 M, and considering the stable viscosity expression of the final modified starch gelatinization solution, the pH of the starch slurry after organic acid treatment was It was found that it was necessary to neutralize with about 5 to 7 and then proceed with water washing and filtration.
이상에서와 같이 본 발명을 상기의 실시예를 통해 설명하였지만 본 발명이 반드시 여기에만 한정되는 것은 아니며 본 발명의 범주와 사상을 벗어나지 않는 범위 내에서 다양한 변형실시가 가능함은 물론이다. 따라서, 본 발명의 보호범위는 본 발명에 첨부된 특허청구의 범위에 속하는 모든 실시 형태를 포함하는 것으로 해석되어야 한다.As described above, the present invention has been described through the above embodiments, but the present invention is not necessarily limited thereto, and various modifications are possible without departing from the scope and spirit of the present invention. Accordingly, the protection scope of the present invention should be construed to include all embodiments falling within the scope of the claims appended hereto.
Claims (8)
상기 중화된 전분 슬러리를 여과, 수세 및 건조하여 수분 함량이 5~15%(w/w)인 유기산 처리 전분을 수득하는 단계; 및
상기 유기산 처리 전분을 밀폐된 용기에 넣고 100~150℃에서 2~20 hr 동안 습열처리하여 최종 변성전분을 수득하는 단계를 포함하는 변성전분 제조방법.
An organic acid was added to the starch slurry to a concentration of 0.05M to 0.5M, and the reaction was carried out at 15 to 55 ° C. for 0.5 to 24 hr. Then, a basic solution was added and the pH of the starch slurry was adjusted to 5 to 7 to obtain a neutralized obtaining a starch slurry;
filtering, washing, and drying the neutralized starch slurry to obtain organic acid-treated starch having a water content of 5 to 15% (w/w); and
A method for producing modified starch comprising the step of obtaining a final modified starch by putting the organic acid-treated starch in a sealed container and subjecting the starch to a wet heat treatment at 100 to 150 ° C. for 2 to 20 hr.
The method of claim 1, wherein the starch concentration in the starch slurry is 20 to 40% by weight based on the dry weight of the starch.
The method according to claim 1, wherein the organic acid is at least one selected from acetic acid, lactic acid, citric acid, and malic acid.
The method according to claim 1, wherein the organic acid is added to the starch slurry at a concentration of 0.08M to 0.4M.
The method for preparing modified starch according to claim 1, wherein the reaction temperature after adding the organic acid is 18 to 30 °C.
The method according to claim 1, wherein the reaction time after adding the organic acid is 1 to 5 hr.
The modified starch according to claim 1, wherein the organic acid-treated starch has a resistant starch content of 30 to 50% and a gelatinization viscosity of 1400 to 2000 centipoise (cPs) at 8% by weight at 50 ° C. manufacturing method.
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