KR100294252B1 - How to increase the content of enzyme resistance starch - Google Patents

How to increase the content of enzyme resistance starch Download PDF

Info

Publication number
KR100294252B1
KR100294252B1 KR1019980026500A KR19980026500A KR100294252B1 KR 100294252 B1 KR100294252 B1 KR 100294252B1 KR 1019980026500 A KR1019980026500 A KR 1019980026500A KR 19980026500 A KR19980026500 A KR 19980026500A KR 100294252 B1 KR100294252 B1 KR 100294252B1
Authority
KR
South Korea
Prior art keywords
starch
content
enzyme
increase
present
Prior art date
Application number
KR1019980026500A
Other languages
Korean (ko)
Other versions
KR20000004816A (en
Inventor
신말식
문세훈
배천호
김은식
최성수
Original Assignee
박종헌
주식회사 삼양제넥스
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 박종헌, 주식회사 삼양제넥스 filed Critical 박종헌
Priority to KR1019980026500A priority Critical patent/KR100294252B1/en
Publication of KR20000004816A publication Critical patent/KR20000004816A/en
Application granted granted Critical
Publication of KR100294252B1 publication Critical patent/KR100294252B1/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/06Drying; Forming

Abstract

본 발명은 전분 분해효소에 대한 저항성을 갖는 전분(효소저항전분)의 함량을 증가시키는 방법에 관한 것으로, 별도의 반복적인 가열-냉각 공정없이, 전분을 압출성형함으로써 효소저항전분의 함량을 증가시키는 방법에 관한 것이다. 본 발명의 방법은 전분을 호화시키기 위하여 필요하였던 반복적인 가열-냉각 공정없이, 또한 가열-냉각 후 건조 공정이 필요없이 압출성형함에 의해 전분 중의 효소저항전분 함량을 증가시킬 수 있으므로 효소저항전분을 제조하기 위한 공정을 단순화시킬 수 있고, 비용을 절약할 수 있다. 또한 압출성형에 의해 최종 제품을 생산하는 경우, 추가 별도의 추가 공정없이 최종 제품 중의 효소저항전분 함량을 증가시킬 수 있다.The present invention relates to a method for increasing the content of starch (enzyme-resistant starch) having resistance to starch degrading enzymes, and to increase the content of enzyme-resistant starch by extrusion molding starch, without a separate repetitive heat-cooling process. It is about a method. Since the method of the present invention can increase the enzyme resistance starch content in the starch by extrusion molding without the repetitive heat-cooling process required for gelatinizing the starch, and without the need for drying after the heat-cooling, the enzyme resistance starch is prepared. The process for doing so can be simplified, and the cost can be saved. In addition, when producing the final product by extrusion molding, it is possible to increase the enzyme resistance starch content in the final product without further additional process.

Description

효소저항전분의 함량을 증가시키는 방법How to increase the content of enzyme resistant starch

본 발명은 전분 분해효소에 대한 저항성을 갖는 전분의 함량을 증가시키는 방법에 관한 것이다.The present invention relates to a method of increasing the content of starch having resistance to starch degrading enzymes.

최근, 기능성 식품에 대한 관심이 높아지면서, 영양생리적으로 활성을 갖는 효소저항전분에 대해 활발한 연구가 진행되고 있다. 본 발명에서, 효소저항전분(resistant starch)은 알파, 베타-아밀라아제 등의 전분 분해효소로 처리하여도 분해되지 않고 남는 전분을 의미한다.Recently, with increasing interest in functional foods, active research is being conducted on enzyme-resistant starches that are nutritionally physiologically active. In the present invention, the resistant starch (starch) refers to starch that remains undecomposed even after treatment with starch degrading enzymes such as alpha and beta-amylase.

이러한 효소저항전분은 식이 섬유소처럼 다이어트 효과를 발휘할 수 있고, 순환계 질환에 대한 예방효과가 있으며 소장에서 소화ㆍ흡수되지 못하고 대장에서 미생물에 의해 발효되어 부티릭산과 같은 단쇄 지방산이 생성되며 이러한 단쇄 지방산은 암세포의 성장을 억제하는 생리적인 기능이 있다고 보고되었다.This enzyme-resistant starch can exert a dietary effect like dietary fiber, prevent circulatory diseases, cannot digest and absorb in the small intestine, ferment by microorganisms in the large intestine, and produce short-chain fatty acids such as butyric acid. It has been reported to have a physiological function of inhibiting the growth of cancer cells.

일반적으로, 전분의 물리, 화학적 처리에 의해 제조된 변성전분은 식품산업에 널리 이용되고 있는데, 인체에 대한 안전성을 고려할 때 화학적인 변성방법보다는 물리적인 변성방법이 더 유용하다.In general, modified starch prepared by physical and chemical treatment of starch is widely used in the food industry, and physical denatured method is more useful than chemical denatured method in consideration of safety to human body.

전분 중의 효소저항전분 함량을 증가시키기 위하여, 전분에 적절한 양의 수분을 첨가하고, 121℃에서 가열한 후 4℃로 냉각하는 과정을 여러 회 반복하면 효소저항전분의 함량이 증가한다고 보고되었다(Sivert.D 등, Cereal Chem. 66 (4), 342-347).In order to increase the content of enzyme-resistant starch in starch, it has been reported that the content of enzyme-resistant starch increases by adding an appropriate amount of water to starch, heating at 121 ° C., and then cooling it to 4 ° C. several times. D et al., Cereal Chem. 66 (4), 342-347).

본 발명자들은 한국특허출원 97-25263에서, 아밀로오스 함량이 10∼40%(w/w)인 전분의 현탁액을 호화온도에서 가열하여 냉각시키고, 이 전분호액을 건조시킨 다음 일정조건하에서 열처리함으로써 효소저항전분의 함량을 증가시키는 방법을 제시하였다. 이 방법에서는 아밀로오스 함량이 10∼40%(w/w)인 아밀로오스 함량이 비교적 낮은 전분을 사용하여서도 효소저항전분 함량이 약 40% 증가하였으나, 수분-열처리 전에, 전분현탁액을 호화온도에서 가열, 냉각하는 과정을 수회 반복하여야 하고 다시 이 전분호액을 건조시켜야 하는 공정이 필요하므로 공정이 번거롭고 제조 시간이 길며, 반복되는 가열 및 냉각 공정에 에너지 소모가 크므로 비용이 많이 소모된다.The inventors of the present invention, in Korean Patent Application 97-25263, a suspension of starch having an amylose content of 10 to 40% (w / w) is heated and cooled at a gelatinization temperature, and the starch solution is dried and then heat treated under a certain condition to enzymatic resistance. A method of increasing the content of starch is presented. In this method, the enzyme resistance starch content was increased by about 40% even when starch with amylose content of 10-40% (w / w) was relatively low, but before the water-heat treatment, the starch suspension was heated at gelatinization temperature, Since the cooling process has to be repeated several times and the starch solution needs to be dried again, the process is cumbersome, the manufacturing time is long, and the energy consumption is high in the repeated heating and cooling processes, which is expensive.

본 발명의 목적은 호화과정을 단순화시키면서도 효소저항전분의 함량을 높일 수 있는, 효소저항전분의 함량을 증가시키는 방법을 제공하는 것이다.An object of the present invention is to provide a method for increasing the content of enzyme-resistant starch, which can increase the content of enzyme-resistant starch while simplifying the gelatinization process.

본 발명의 목적은 효소저항전분 함량이 증가된 식품을 제공한다.It is an object of the present invention to provide foods with increased enzyme resistance starch content.

본 발명은 별도의 전처리 없이 압출성형공정에 의해 효소저항전분의 함량의 증가시킬 수 있음을 제시한다.The present invention suggests that it is possible to increase the content of the enzyme resistance starch by the extrusion molding process without a separate pretreatment.

본 발명의 방법은 전분을 함유하는 식품 재료를 압출성형하는 것으로 이루어진다.The method of the present invention consists in extruding a food material containing starch.

전분은 그 자체로뿐 아니라, 전분에 물리적, 화학적 처리를 하여 적절한 성질을 갖는 변성 전분을 만들어 식품 산업에 응용하고 있다. 한 예로, 압출성형 역시 변성전분 제조에 응용될 수 있는데 최근 식품 가공공정 중 예를 들어 스낵류 등의 제조에 압출성형 공정의 이용이 증가되고 있다.Starch is applied to the food industry not only by itself, but also by physically and chemically treating starch to make modified starch having proper properties. For example, extrusion may also be applied to the production of modified starch. Recently, the use of the extrusion process has been increased in the food processing process, for example, in the production of snacks.

본 발명에 따르면, 종래 방법에 따라 효소저항전분을 제조하기 위하여 필요하였던 호화공정, 즉 전분에 수분을 가한 후 100∼130℃에서 가열하고 냉각시키는 가열ㆍ냉각 공정을 2∼6회 반복하고 또 이렇게 하여 얻어진 전분 페이스트를 다시 건조하는 공정을 거칠 필요 없이, 단순히 원료전분을 압출성형함에 의해 전분 중의 효소저항전분의 함량을 증가시킬 수 있으므로 공정을 단순화할 수 있을 뿐 아니라 가열ㆍ냉각 공정을 반복하는데 필요한 에너지를 절감할 수 있어 효소저항전분 제조 비용을 줄일 수 있다.According to the present invention, the gelatinization process required for preparing enzyme-resistant starch according to the conventional method is repeated two to six times, that is, the heating and cooling process of adding water to the starch and heating and cooling it at 100 to 130 ° C. It is possible to increase the content of the enzyme-resistant starch in the starch by simply extruding the raw starch, without having to go through the process of drying the starch paste obtained by the step again, thereby simplifying the process and repeating the heating and cooling process. Energy can be saved, reducing the production cost of enzyme-resistant starch.

본 발명의 방법에서, 추가로, 압출성형 후 압출성형된 시료를 열처리할 수 있다. 열처리 방법 및 조건은 한국특허출원 97-25263에 기재된 내용을 참고할 수 있는데, 예를 들어, 압출성형된 시료를 100∼130℃에서 가열하고 냉각시키는 가열ㆍ냉각 공정을 1∼6회 반복한다. 이와 같이 본 발명의 방법에서는 압출성형된 시료를 특별히 건조할 필요없이, 필요한 경우 수분을 첨가하거나 또는 첨가하지 않고 단순히 열처리함으로써 최종 제품 중의 효소저항 전분의 함량을 더욱 증가시킬 수 있다.In the process of the invention, further, the extruded sample may be heat treated after extrusion. The method and conditions for the heat treatment can be referred to the contents described in Korean Patent Application No. 97-25263. For example, the heating and cooling process of heating and cooling the extruded sample at 100 to 130 ° C. is repeated 1 to 6 times. As such, the method of the present invention can further increase the content of the enzyme-resistant starch in the final product by simply heat treatment with or without adding water, if necessary, without particularly drying the extruded sample.

본 발명의 방법에서는 압출성형 조건을 조절함으로써 효소저항전분의 함량을 조절할 수 있다. 압출성형시 원료전분에 첨가하는 수분량은 크게 한정되지는 않으나, 압출성형 후 노화가 촉진될 수 있는 수분량, 예를 들어 건조 전분에 대해 0%∼50%(w/w), 바람직하게는 15%∼25%(w/w)되도록 첨가할 수 있다.In the method of the present invention, it is possible to control the content of the enzyme resistance starch by controlling the extrusion molding conditions. The amount of water added to the raw starch during extrusion is not limited, but the amount of moisture that may accelerate aging after extrusion, for example, 0% to 50% (w / w) for dry starch, preferably 15% It may be added so as to be ˜25% (w / w).

본 발명에서, 압출성형으로 얻어진 제품은 종래의 방법에 따라 열풍에 의해 건조시킬 수 있다.In the present invention, the product obtained by extrusion molding can be dried by hot air according to a conventional method.

본 발명의 방법에서, 추가로, 압출성형된 시료를 저온 처리할 수 있다. 저온 처리는 약 -10∼20℃에 일정시간 방치하는 것으로 이루어진다. 저온처리 시간은 특별히 한정되지 않으며, 시료의 종류, 시료 양, 최종 제품의 수분 함량 등에 따라 적절한 시간을 선택한다. 이와 같이 저온처리함으로써 제품이 건조되는 동시에 노화가 진행되므로 최종 제품 중의 효소저항전분의 함량을 증가시킬 수 있다.In the process of the invention, further, the extruded sample can be cold treated. Low temperature treatment consists of leaving it to stand at about -10-20 degreeC for a fixed time. The low temperature treatment time is not particularly limited, and an appropriate time is selected according to the type of sample, the amount of the sample, and the water content of the final product. As a result of the low temperature treatment, the product is dried and at the same time, the aging proceeds, thereby increasing the content of enzyme-resistant starch in the final product.

본 발명은 효소저항전분의 함량이 증가된 변성전분을 제조하기 위해 이용될 수 있으며, 또한 스낵류와 같은 최종 제품을 생산하는데 이용될 수 있다.The present invention can be used to produce modified starch with increased content of enzyme resistant starch, and can also be used to produce final products such as snacks.

본 발명에서 전분은 옥수수전분, 감자전분, 고구마전분, 타피오카 전분, 사고전분, 쌀전분, 밀전분, 동부전분 등을 사용할 수 있다.In the present invention, the starch may be used corn starch, potato starch, sweet potato starch, tapioca starch, sago starch, rice starch, wheat starch, eastern starch.

본 명세서에서 효소저항전분 함량은 다음에 기재된 효소-중량법에 의하여 측정하였다.The enzyme resistance starch content herein was measured by the enzyme-weight method described below.

효소저항전분의 분리 및 함량 측정Separation and Measurement of Enzyme Resistance Starch

제조된 시료 1g과 인산완충용액(pH 6.0) 50ml를 비이커에 넣고, 내열성 알파 아밀라제 0.1ml를 첨가하여, 끓는 항온수조에서 30분간 반응시킨 다음, 실온까지 용액을 냉각시켜 0.275N 가성소다로 pH를 7.5로 조정한다. 이 용액에, 50mg의 프로테아제를 1ml의 인산완충용액에 분산시킨 용액 0.1ml를 첨가하여 60℃에서 30분동안 흔들면서 반응시켰고, 다시 실온까지 냉각시켜 0.325N 염산으로 pH가 4.3이 되도록 조정한 다음, 아밀로글루코시다제 0.3ml를 첨가하여 60℃에서 30분동안 흔들면서 반응시켰다. 그런 다음, 용액의 최종 알코올 농도가 80%(v/v)되게 에탄올을 첨가하고 여과지(Whatman No. 1)를 사용하여 여과한 후, 아세톤으로 세척하고 불용성 잔사를 실온에서 하루 방치하여 건조시켜 무게를 측정하였다. 효소저항전분의 함량은 다음과 같이 산출하였다.1 g of the prepared sample and 50 ml of phosphate buffer solution (pH 6.0) were added to a beaker, and 0.1 ml of heat-resistant alpha amylase was added thereto. The reaction was carried out in a boiling water bath for 30 minutes, and then the solution was cooled to room temperature and the pH was adjusted to 0.275 N caustic soda. Adjust to 7.5. To this solution, 0.1 mg of a solution of 50 mg of protease dispersed in 1 ml of phosphate buffer solution was added and reacted by shaking at 60 ° C. for 30 minutes, cooled to room temperature, and adjusted to pH 4.3 with 0.325 N hydrochloric acid. 0.3 ml of amyloglucosidase was added and reacted with shaking at 60 ° C. for 30 minutes. Then, add ethanol so that the final alcohol concentration of the solution is 80% (v / v), filter using filter paper (Whatman No. 1), wash with acetone and leave insoluble residue at room temperature for one day to dry Was measured. The content of enzyme resistance starch was calculated as follows.

효소저항정분의 함량(%(w/w))=불용성 잔사의 무게(g)/시료의 무게(g)x100Enzyme Resistance Content (% (w / w)) = Weight of Insoluble Residue (g) / Weight of Sample (g) x 100

이하, 본 발명을 실시예에 의하여 더욱 구체적으로 설명하고자 한다. 이들 실시예는 오로지 본 발명을 구체적으로 설명하는 것으로, 이들 실시예에 의해 본 발명의 범위가 제한되지 않는다는 것은 당업계에서 통상의 지식을 가진 자들에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only to specifically describe the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples.

실시예 1Example 1

아밀로스 함량이 약 23%(w/w)인 옥수수 전분과 약 70%(w/w)인 옥수수 전분을 단축압출성형기(공주대학교 식품공학과, 예산)를 사용하여, 표 1의 조건으로 압출성형하였다. 압출성형으로 얻어진 페이스트를 표 1의 조건으로 40℃에서 열풍건조시키거나 또는 4℃에서 냉장시키고 마쇄한 후 효소-중량법에 의하여 효소저항전분을 분리하고 수율을 측정하였다. 건조된 시료를 마쇄한 후 100 메쉬체를 통과시켰다. 앞에 기재된 효소-중량법에 의하여 효소저항전분을 분리하고 수율을 측정하였다. 결과를 표 1에 나타낸다.Corn starch with amylose content of about 23% (w / w) and corn starch with about 70% (w / w) were extruded under the conditions of Table 1 using a single extrusion extruder (Dept. of Food Science and Technology, Kongju National University). . The paste obtained by extrusion molding was hot-air dried at 40 ° C. or refrigerated at 4 ° C. and crushed. The enzyme resistance starch was separated by enzyme-weight method and the yield was measured. After the dried sample was ground, a 100 mesh sieve was passed. Enzyme-resistant starch was isolated by the enzyme-weight method described above and the yield was measured. The results are shown in Table 1.

[표 1]TABLE 1

본 발명의 방법은 전분을 호화시키기 위하여 필요하였던 반복적인 가열-냉각 공정없이, 또한 가열-냉각 후 건조 공정이 필요없이 압출성형함에 의해, 또는 압출성형 후 저온처리함에 의해 전분 중의 효소저항전분 함량을 증가시킬 수 있으므로 효소저항전분을 제조하기 위한 공정을 단순화시킬 수 있고, 비용을 절약할 수 있다. 또한 압출성형에 의해 최종 제품을 생산하는 경우, 별도의 추가 공정없이 최종 제품 중의 효소저항전분 함량을 증가시킬 수 있다.The process of the present invention provides a method for reducing the content of enzyme resistance starch in starch by extrusion without the repetitive heat-cooling process required for gelatinizing the starch, and without the need for drying after heat-cooling, or by cold treatment after extrusion. As a result, the process for preparing enzyme-resistant starch can be simplified, and the cost can be saved. In addition, when the final product is produced by extrusion molding, it is possible to increase the enzyme resistance starch content in the final product without additional processing.

Claims (3)

전분에 별도의 화학적 처리 없이, 수분함량이 10-50%(w/w)인 전분을 80℃∼150℃의 온도에서 압출하는 것으로 이루어지는, 효소저항전분의 함량을 증가시키는 방법.A method for increasing the content of enzyme-resistant starch, comprising extruding starch having a water content of 10-50% (w / w) at a temperature of 80 ° C to 150 ° C without any chemical treatment. 제1항에 있어서, 압출한 전분을 추가로 100℃∼150℃의 온도에서 가열하는 것을 특징으로 하는 방법.The method according to claim 1, wherein the extruded starch is further heated at a temperature of 100 ° C to 150 ° C. 제1항에 있어서, 압출한 전분을 -10℃∼-20℃에서 일정시간 방치하는 것을 특징으로 하는 방법.The method according to claim 1, wherein the extruded starch is left at -10 ° C to -20 ° C for a predetermined time.
KR1019980026500A 1998-06-30 1998-06-30 How to increase the content of enzyme resistance starch KR100294252B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019980026500A KR100294252B1 (en) 1998-06-30 1998-06-30 How to increase the content of enzyme resistance starch

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019980026500A KR100294252B1 (en) 1998-06-30 1998-06-30 How to increase the content of enzyme resistance starch

Publications (2)

Publication Number Publication Date
KR20000004816A KR20000004816A (en) 2000-01-25
KR100294252B1 true KR100294252B1 (en) 2001-10-27

Family

ID=19542769

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1019980026500A KR100294252B1 (en) 1998-06-30 1998-06-30 How to increase the content of enzyme resistance starch

Country Status (1)

Country Link
KR (1) KR100294252B1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113679053A (en) * 2021-08-13 2021-11-23 江南大学 Low-glycemic starch derivative and processing method thereof

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030067894A (en) * 2002-02-08 2003-08-19 동아제분 주식회사 Wheat flour premix composition for cookie and cake
KR102055983B1 (en) 2017-11-10 2019-12-13 김양희 The Mixture for manufacturing of companion animal feeds having in blood sugar level

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5472732A (en) * 1991-10-17 1995-12-05 Matsutani Chemical Industries Co., Ltd. Indigestible dextrin

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5472732A (en) * 1991-10-17 1995-12-05 Matsutani Chemical Industries Co., Ltd. Indigestible dextrin

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113679053A (en) * 2021-08-13 2021-11-23 江南大学 Low-glycemic starch derivative and processing method thereof

Also Published As

Publication number Publication date
KR20000004816A (en) 2000-01-25

Similar Documents

Publication Publication Date Title
AU766960B2 (en) Method for producing resistant starch
Mercier Effect of extrusion‐cooking on potato starch using a twin screw French extruder
Zhao et al. The impact of coupled acid or pullulanase debranching on the formation of resistant starch from maize starch with autoclaving–cooling cycles
KR20080023674A (en) Production of enzyme-resistant starch by extrusion
AU2007201065B2 (en) Process tolerant starch composition with high total dietary fiber content
JP2001231469A (en) Highly resistant granular starch
KR20090121313A (en) Production of resistant starch product
Lehmann et al. Production and physicochemical characterization of resistant starch type III derived from pea starch
AU2003204157A1 (en) Resistant starch prepared by isoamylase debranching of low amylose starch
WO2019114020A1 (en) Modification method for improving slow digestion performance of starch
Zhao et al. Resistant starch prepared from high-amylose maize starch with citric acid hydrolysis and its simulated fermentation in vitro
KR100936590B1 (en) Continuous Process for Modifying Starch and Its Derivatives by Branching Enzymes
KR101145375B1 (en) Resistant starch with high viscosity and manufacturing method of the same
Górecki et al. Influence of high pressure or autoclaving-cooling cycles and pullulanase treatment on buckwheat starch properties and resistant starch formation
KR100294252B1 (en) How to increase the content of enzyme resistance starch
Wong et al. Enzymatic production of linear long-chain dextrin from sago (Metroxylon sagu) starch
US20220408766A1 (en) Method for annealing pea starch
Abioye et al. Effect of autoclaving on the formation of resistant starch from two Nigeria Cassava (Manihot esculenta) varieties
KR101068986B1 (en) Resistant starch with pasting properties and manufacturing method of the same
KR100411510B1 (en) Method for increasing resistant starch by addition of nonvolatile organic acid
KR100218232B1 (en) Method of increasing starch which is resistant to starch degrading enzyme
EP1429626A1 (en) Enzymatic treatment of starchy food products for shortening the tempering step
US10392640B2 (en) Method for modifying starch to slow down the digestion rate
Wilkins et al. Variability of reaction efficiencies and pasting properties of acetylated dent corn starch from various commercial hybrids
Liu et al. Pea resistant starch preparation with cold-active type I pullulanase from Bacillus megaterium and its potential application in rice noodles

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
N236 Change of applicant [patent]: notification of change of applicant and registration of partial transfer of right
FPAY Annual fee payment

Payment date: 20130227

Year of fee payment: 13

FPAY Annual fee payment

Payment date: 20140312

Year of fee payment: 14

FPAY Annual fee payment

Payment date: 20160304

Year of fee payment: 16

FPAY Annual fee payment

Payment date: 20170306

Year of fee payment: 17

LAPS Lapse due to unpaid annual fee