KR100505532B1 - Process for preparing succinylated gelatin - Google Patents
Process for preparing succinylated gelatin Download PDFInfo
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- KR100505532B1 KR100505532B1 KR10-2003-0061317A KR20030061317A KR100505532B1 KR 100505532 B1 KR100505532 B1 KR 100505532B1 KR 20030061317 A KR20030061317 A KR 20030061317A KR 100505532 B1 KR100505532 B1 KR 100505532B1
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- gelatin
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- succinic
- alkali
- acid treatment
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 108010013480 succinylated gelatin Proteins 0.000 title 1
- 229940007079 succinylated gelatin Drugs 0.000 title 1
- 108010010803 Gelatin Proteins 0.000 claims abstract description 83
- 229920000159 gelatin Polymers 0.000 claims abstract description 83
- 239000008273 gelatin Substances 0.000 claims abstract description 83
- 235000019322 gelatine Nutrition 0.000 claims abstract description 83
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 83
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000010306 acid treatment Methods 0.000 claims abstract description 19
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 15
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 241000251468 Actinopterygii Species 0.000 claims abstract description 11
- 239000001384 succinic acid Substances 0.000 claims abstract description 7
- 238000006482 condensation reaction Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 8
- 229940014800 succinic anhydride Drugs 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000001954 sterilising effect Effects 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 5
- 238000004659 sterilization and disinfection Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 36
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 16
- 125000003277 amino group Chemical group 0.000 description 9
- 239000002775 capsule Substances 0.000 description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 8
- 238000006467 substitution reaction Methods 0.000 description 6
- 125000003172 aldehyde group Chemical group 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 4
- 230000003111 delayed effect Effects 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 241000283690 Bos taurus Species 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 235000015278 beef Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007903 gelatin capsule Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000825 pharmaceutical preparation Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 235000015277 pork Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical compound N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000005882 aldol condensation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- OVYQSRKFHNKIBM-UHFFFAOYSA-N butanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)CCC(O)=O OVYQSRKFHNKIBM-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000019645 odor Nutrition 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000019617 pupation Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin or cold insoluble globulin [CIG]
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/02—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length in solution
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/145—Extraction; Separation; Purification by extraction or solubilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K19/00—Hybrid peptides, i.e. peptides covalently bound to nucleic acids, or non-covalently bound protein-protein complexes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Analytical Chemistry (AREA)
- Toxicology (AREA)
- Zoology (AREA)
- Gastroenterology & Hepatology (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
본 발명은 우피(Hide Splits), 돈피 (Pig Skin), 건조된 소뼈(Ossein),어류를 원료로 사용하여 알칼리 처리, 산 처리, 알칼리 및 산 처리를 하는 3단계 전처리 공정 ; 추출 반응조에서 상기 전처리 공정을 거친 원료를 통해 젤라틴을 추출하는 공정 ; 상기 추출된 젤라틴 용액을 수산화나트륨 수용액으로 pH 7.0∼8.0으로 조절하면서 무수 호박산을 첨가 축합 반응시켜 호박산 젤라틴을 제조하는 공정 ; 상기 호박산 젤라틴 용액을 여과 농축 건조시키는 공정을 포함함을 특징으로 하는 호박산 젤라틴의 제조방법을 제공하는 것이다.The present invention is a three-stage pretreatment process using an alkali treatment, acid treatment, alkali and acid treatment using Hide Splits, Pig Skin, dried Ossein, fish as raw materials; Extracting gelatin through a raw material that has undergone the pretreatment step in an extraction reactor; Preparing a succinic gelatin by adding condensation reaction of the extracted gelatin solution with an aqueous sodium hydroxide solution to pH 7.0 to 8.0 while adding condensed anhydrous succinic acid; It provides a method for producing succinic gelatin, characterized in that it comprises a step of filtering and drying the succinic gelatin solution.
Description
본 발명은 우피, 돈피, 건조된 소뼈, 어류 등의 다양한 원료를 이용하여 천연 젤라틴을 추출한 후, 상기 추출된 젤라틴 용액에 무수 호박산을 첨가 반응시켜 호박산 젤라틴을 제조하는 제조방법에 관한 것이다.The present invention relates to a method for producing succinic gelatin by extracting natural gelatin using various raw materials such as cowhide, pork skin, dried bovine bone, fish, and then adding succinic anhydride to the extracted gelatin solution.
더욱 상세하게는, 우피(Hide Splits), 돈피(Pig Skin), 건조된 소뼈(Ossein), 어류를 원료로 사용하여 알칼리 처리, 산 처리, 알칼리 및 산 처리 공정을 포함하는 3단계 전처리 공정 후, 추출 반응조에서 젤라틴을 추출하고, 상기 추출된 젤라틴 용액에 무수 호박산을 첨가 축합 반응시켜 호박산 젤라틴을 제조한 후, 제조된 호박산 젤라틴을 여과 농축 건조시키는 공정을 포함하는 호박산 젤라틴의 제조방법에 관한 것이다.More specifically, after a three-stage pretreatment process including alkali treatment, acid treatment, alkali and acid treatment using hide splits, pig skin, dried ossein and fish as raw materials, The present invention relates to a method for producing succinic gelatin, which comprises extracting gelatin in an extraction reactor, adding condensation reaction of succinic anhydride to the extracted gelatin solution to prepare succinic gelatin, and then filtering and drying the succinate gelatin.
일반 젤라틴에 호박산을 첨가 반응시켜 호박산 젤라틴을 제조하는 반응 메카니즘을 살펴보면 다음과 같다.The reaction mechanism for preparing succinic gelatin by adding succinic acid to the normal gelatin is as follows.
일반 젤라틴 무수 호박산 호박산 젤라틴 Normal gelatin Anhydrous succinate succinate gelatin
즉 호박산 젤라틴은 일반 젤라틴의 아미노기(-NH3 +)를 숙시닐화(succinic) 시켜 카르복실기(-COOH)로 치환시킨 형태의 화학적 구조를 지니는 것으로 일반 젤라틴에 비해 캡슐로 만들었을 때, 붕해성이 일반 젤라틴 보다 월등히 우수하다.In other words, succinate gelatin has a chemical structure in which the amino group (-NH 3 + ) of normal gelatin is succinylated and substituted with a carboxyl group (-COOH). It is much better than gelatin.
일반 젤라틴으로 제조된 캡슐은 내용물이 특수한 약물의 경우, 특히 알데히드기(-CHO)를 함유한 것인 경우 일반 젤라틴의 아미노기(-NH3 +)와 용이하게 반응하여 알데히드로 난용화 되거나, 자체 축합 반응을 일으켜 케톤의 화합물로 거대분자를 형성하는 것으로 알려져 있다.In the case of the capsule contents are special manufacturing drugs to normal gelatin, especially not containing an aldehyde group (-CHO) to readily react with the amino group (-NH 3 +) common gelatin I with an aldehyde or pupation, self-condensation reaction It is known to form macromolecules with compounds of ketones.
그런데 이와 같은 젤라틴 거대 분자 형성은 제품으로 되어진 캡슐의 불용성이라는 성질을 야기시켜 약전에 규정된 붕해 시간 내에 충분히 붕해되지 못하는 결점을 초래하였다. 특히 장기간 보관을 하였을 경우 이러한 현상의 발생으로 좋지 않은 결과를 나타내기도 한다. 그러나 호박산 젤라틴은 일반 젤라틴의 아미노기(-NH3 +)가 카르복실기(-COOH)로 치환되어 있어 알데히드 및 케톤화 반응이 적게 일어나 부반응으로 인한 붕해성의 저하를 야기시키지 않는다.Such gelatinous macromolecular formation, however, causes the insoluble nature of the capsules to be made into products, resulting in a defect that cannot be sufficiently disintegrated within the disintegration time specified in the pharmacopoeia. In particular, long-term storage may cause unfavorable results. However, succinate gelatin has less aldehyde and ketoneization reaction because the amino group (-NH 3 + ) of general gelatin is substituted with carboxyl group (-COOH), and thus does not cause degradation of disintegration due to side reactions.
아래는 일반 젤라틴으로 만든 캡슐의 붕해 지연 이유를 구체적으로 서술한 것이다.Below is a detailed explanation of the reason for the delayed disintegration of capsules made with normal gelatin.
의약제재 성분 중에 포함된 알데히드기(-CHO)와 일반 젤라틴의 아미노 그룹이 알돌 축합(Aldol Condensation) 반응을 일으켜 거대분자를 형성함으로써 붕해 지연을 일으키는 것이다.The aldehyde group (-CHO) contained in the pharmaceutical ingredient and the amino group of general gelatin cause an Aldol condensation reaction to form macromolecules, causing disintegration delay.
젤라틴 자체 축합 반응에 의해 붕해를 지연시킬 수도 있다. 즉 일반 젤라틴 자체의 아미노기(-NH3 +)와 카르복시기(-COOH)가 반응하여 아미드(amide)결합을 형성하여 붕해 지연을 일으키는 원인이 있다.Disintegration may also be delayed by gelatin self-condensation reactions. That is, the amino group (-NH 3 + ) of the general gelatin itself and the carboxy group (-COOH) react to form an amide (amide) bond, causing a disintegration delay.
한편 활성 성분의 산화에 의한 붕해 지연도 가능한 바, 하이드록실기(-OH)를 가지고 있는 의약품 제재의 경우 산화에 의하여 알데히드기가 형성되고 이 알데히드기와 젤라틴의 아미노그룹이 카보닐아민(Carbonylamine)반응을 통하여 교차결합(Cross-linking)을 일으켜 붕해를 지연시킬 수 있다.On the other hand, the disintegration may be delayed due to the oxidation of the active ingredient. In the case of a pharmaceutical product having a hydroxyl group (-OH), an aldehyde group is formed by oxidation, and the amino group of the aldehyde group and gelatin undergoes a carbonylamine reaction. Cross-linking can be used to delay disintegration.
의약품 제재가 탄닌 계열의 화합물인 경우 이에 따른 붕해 지연도 가능하며, 대부분의 식물 엑기스는 F. Tannis을 가지고 있으므로 시간 경과에 따라 F. Tannis는 젤라틴의 아미노 그룹과 반응하여 붕해 지연을 일으킨다.If the pharmaceutical formulation is a tannin-based compound, disintegration may be delayed. Since most plant extracts have F. Tannis, over time, F. Tannis reacts with the amino group of gelatin to cause disintegration delay.
마지막으로 캡슐 내에 함유된 가소제 산화에 의한 붕해 지연도 야기될 수 있고, 즉 가소제인 글리세린 등의 하이드록실기(-OH)의 산화에 의해 알데히드기(-CHO)가 생성되어 젤라틴의 아미노 그룹과 반응하여 붕해 지연을 일으키는 것이다.Finally, the disintegration delay may be caused by the oxidation of the plasticizer contained in the capsule, that is, the oxidation of hydroxyl group (-OH) such as glycerin, a plasticizer, generates an aldehyde group (-CHO) and reacts with the amino group of gelatin. Causing disintegration delay.
상기와 같은 통상의 젤라틴을 이용한 캡슐제의 붕해도 저하를 방지하기 위해서는 젤라틴을 호박산 젤라틴으로 대체시켜 캡슐제를 제조하는 것이 바람직하며 본 발명은 이와 같은 캡슐제의 원료로 사용하기 위한 호박산 젤라틴의 개량된 제조방법을 제공하는 것이다.In order to prevent the disintegration of the capsule using the conventional gelatin as described above, it is preferable to prepare a capsule by replacing the gelatin with succinate gelatin, and the present invention is an improvement of the succinate gelatin for use as a raw material of such a capsule. It is to provide a manufactured method.
따라서 본 발명이 이루고자 하는 기술적 과제는 붕해성 지연 문제를 일으키는 일반 젤라틴의 아미노기(-NH3 +)를 카르복실기(-COOH)로 치환(Succinic화)시켜 특정 의약품 제재와의 알데히드 및 케톤화 반응을 방지할 수 있는 호박산 젤라틴을 개발·적용하여 캡슐의 경시 변화에 따른 용해성과 붕해성 문제를 해결하는데 그 목적이 있다.Therefore, the technical problem to be achieved by the present invention is to prevent the aldehyde and ketoneization reaction with certain pharmaceutical preparations by replacing (succinic) the amino group (-NH 3 + ) of the general gelatin causing a disintegration delay problem with a carboxyl group (-COOH) The purpose is to solve the solubility and disintegration problem caused by the change of capsules over time by developing and applying succinic gelatin.
따라서 본 발명은 우피(Hide Splits), 돈피 (Pig Skin), 건조된 소뼈(Ossein),어류를 원료로 사용하여 알칼리 처리, 산 처리, 알칼리 및 산 처리를 하는 3단계 전처리 공정 ; 추출 반응조에서 상기 전처리 공정을 거친 원료를 통해 젤라틴을 추출하는 공정 ; 상기 추출된 젤라틴 용액을 수산화나트륨 수용액으로 pH 7.0∼8.0으로 조절하면서 무수 호박산을 첨가 축합 반응시켜 호박산 젤라틴을 제조하는 공정 ; 상기 호박산 젤라틴 용액을 여과 농축 건조시키는 공정을 포함함을 특징으로 하는 호박산 젤라틴의 제조방법을 제공하는 것이다.Therefore, the present invention comprises a three-stage pretreatment process of using an alkali treatment, acid treatment, alkali and acid treatment using hide splits, pig skin, dried beef bones and fish as raw materials; Extracting gelatin through a raw material that has undergone the pretreatment step in an extraction reactor; Preparing a succinic gelatin by adding condensation reaction of the extracted gelatin solution with an aqueous sodium hydroxide solution to pH 7.0 to 8.0 while adding condensed anhydrous succinic acid; It provides a method for producing succinic gelatin, characterized in that it comprises a step of filtering and drying the succinic gelatin solution.
이 때 상기 전처리 공정 중 알칼리 처리 시간은 24∼48시간이고 산 처리 시간은 18∼28 시간이며, 추출 온도는 45∼55℃, 추출조의 물 추출시간은 6∼10 시간이며, 추출액의 젤라틴 농도 4∼6 (w/v)% 임을 특징으로 하고, 추출액의 pH를 7.0∼8.0으로 조절하면서 상기 추출 젤라틴 용액에 대하여 동일 농도(4∼6 (w/v)%)의 무수 호박산을 첨가 반응시킴을 특징으로 하고, 상기 여과 공정은 펄프로 1, 2차 여과시키고 카본 필터로 3차 여과시켜 추출 용액의 취미를 제거시킴을 특징으로 한다.At this time, the alkali treatment time in the pretreatment process is 24 to 48 hours, the acid treatment time is 18 to 28 hours, the extraction temperature is 45 to 55 ° C, the extraction time of the water to the extraction tank is 6 to 10 hours, and the gelatin concentration of the extract 4 ˜6 (w / v)% of the extract, and reacting the extracted gelatin solution with the same concentration (4-6 (w / v)%) of anhydrous succinic acid while adjusting the pH of the extract to 7.0-8.0. The filtration process is characterized in that the first and second filtration with pulp and third filtration with a carbon filter to remove the hobby of the extraction solution.
한편, 상기 농축 공정은 2단계 멤브레인 시스템을 거쳐 농축시키고, 농축 후 142℃ 이상에서 살균 공정을 포함함을 특징으로 한다.On the other hand, the concentration process is characterized in that the concentration through a two-stage membrane system, and after the concentration includes a sterilization process at 142 ℃ or more.
이하 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명은 우피(Hide Splits), 돈피(Pig Skin), 건조된 소뼈(Ossein), 어류로부터 알칼리 처리, 산 처리, 알칼리와 산 처리를 겸한 3단계 전처리 공정 후, 추출조에서 추출하는 것으로 4∼6%의 젤라틴 용액에 대하여 무수 호박산 4∼6 중량%를 pH 7.0∼8.0으로 조절하면서 첨가 반응시킨 후 여과, 농축, 살균, 건조하는 공정이다.The present invention is to extract from the extraction tank after a three-stage pretreatment process, including alkali treatment, acid treatment, alkali and acid treatment from Hide Splits, Pig Skin, dried Ossein, fish It is a process of adding, reacting 4-6 weight% of succinic anhydride to pH 7.0-8.0 with respect to 6% gelatin solution, and filtering, concentrating, sterilizing, and drying.
전처리 공정에 있어 알칼리 처리는 수산화나트륨 수용액(pH 12.5∼13.6)에서 24∼48시간 처리하고, 산 처리는 염산 수용액(pH 1.5∼2.5)에서 18∼28시간 처리 한 다음 pH가 4.5∼5.0이 될 때까지 충분한 물을 공급하면서 세척을 실시한다. 수세 과정에서 원료에 잔류해 있는 불순물 및 과잉의 알칼리와 산을 최종적으로 제거하고 젤라틴 추출에 적합한 원료 상태를 만들어 준다.In the pretreatment process, alkali treatment is performed for 24 to 48 hours in an aqueous sodium hydroxide solution (pH 12.5 to 13.6), and acid treatment is for 18 to 28 hours in an aqueous hydrochloric acid solution (pH 1.5 to 2.5), and the pH becomes 4.5 to 5.0. Wash with sufficient water until In the washing process, impurities and residual alkali and acid remaining in the raw material are finally removed and the raw material is suitable for gelatin extraction.
전처리 된 원료는 추출조에서 추출온도 45∼55℃, 추출시간 6∼10시간 동안 추출한 후 젤라틴 농도가 4∼6%가 되면 드레인 하여 무수 호박산을 첨가 반응시킨다.The pretreated raw material is extracted in extraction tank for 45 ~ 55 ℃ and extraction time for 6 ~ 10 hours, and then drained when gelatin concentration reaches 4 ~ 6%.
무수 호박산 첨가 반응시 젤라틴 용액의 농도는 4∼6%이며 수산화나트륨 수용액(순도 33%)을 이용하여 젤라틴 용액의 pH를 7.0∼8.0으로 조절하면서 상기 젤라틴에 대하여 무수 호박산 4∼6%를 동시에 투입한다. When the anhydrous succinic acid is added, the concentration of gelatin solution is 4-6%, and 4-6% of succinic anhydride is simultaneously added to the gelatin while the pH of the gelatin solution is adjusted to 7.0-8.0 using an aqueous sodium hydroxide solution (purity 33%). do.
반응이 완료된 호박산 젤라틴 용액은 1차 여과 공정을 거쳐 이온교환수지탑에서 미네랄 성분이 제거된 후, 멤브레인 시스템을 통과하여 6%인 용액이 12%까지 농축되고 2, 3차 여과공정을 다시 통과한 후 스팀을 이용한 진공 농축 공정을 거친다.After completion of the reaction, the succinate gelatin solution is subjected to the first filtration process to remove the minerals from the ion exchange resin tower, and then through the membrane system, 6% of the solution is concentrated to 12% and passed through the second and third filtration processes again. After the vacuum concentration process using steam.
스팀을 이용한 진공 농축 전에 용액을 2단계에 걸쳐 멤브레인을 통과시켜 6%인 용액의 농도를 12%까지 농축시킴으로써 스팀 등 외부의 에너지를 이용하지 않고 자연 농축이 가능하여 물성 보호가 가능하며, 사전 12%까지 농축시킴으로써 진공 농축 공정에서도 적은 에너지로 물성 변화를 최소화시키면서 농축이 가능하다.The solution is passed through the membrane in two stages prior to vacuum concentration using steam to concentrate the concentration of 6% solution to 12%, allowing natural concentration without using external energy such as steam. By concentrating up to%, even in a vacuum condensation process, it is possible to concentrate while minimizing physical property changes with less energy.
30∼35%로 농축된 용액이 최종 살균공정을 통과하기 전에 카본 필터 시스템을 통과시킴으로써, 젤라틴에서 발생될 수 있는 취미를 산화제나, 화학약품을 전혀 사용치 않고 완벽한 이취 제거 및 극미세 이물제거가 가능하다는 것이다.By passing through a carbon filter system before the solution is concentrated to 30-35%, the hobby that can be generated in gelatin is completely eliminated with no oxidizing agents or chemicals, and is completely free of odors. It is possible.
마지막 살균 공정에서는 142℃의 초고온에서 6∼7초간 순간 살균을 실시함으로써 젤라틴 내의 세균을 사멸시킬 수 있다.In the last sterilization process, microorganisms in the gelatin can be killed by instant sterilization at an extremely high temperature of 142 ° C. for 6 to 7 seconds.
따라서 본 발명은 우피, 돈피, 건조된 소뼈, 어류를 알칼리 처리, 산 처리, 알칼리 및 산 처리를 하는 3단계의 전처리 공정을 통하여 추출된 젤라틴 용액에 무수 호박산을 첨가 반응시킴으로써 붕해성이 뛰어난 호박산 젤라틴을 제조할 수 있었다.Therefore, the present invention is a succinic gelatin excellent in disintegration by adding succinic anhydride to the gelatin solution extracted through the three-step pretreatment process of the cow skin, pork skin, dried beef bones, alkali treatment, acid treatment, alkali and acid treatment Could be prepared.
이와 같은 본 발명은 실시예에 의거하여 상세하게 설명한다. 그러나 본 발명의 범위가 하기 실시예에 의해 한정되는 것은 아니다.This invention is demonstrated in detail based on an Example. However, the scope of the present invention is not limited by the following examples.
(실시예 1)(Example 1)
정제수 10L에 수산화나트륨 용액(순도 33%)을 443㎖을 넣어서 pH 13.4의 알칼리 수용액을 제조한다. 여기서 수분함량 14%인 건조된 어류 비늘을 교반기를 가동시키면서 1.0㎏ 투입한 후 교반기를 계속 가동시키면서 36시간 지속시킨다. 이러한 알칼리 처리가 종료된 후 알칼리수는 완전히 Drain시킨 후 10L 씩의 정제수로 약 30분씩 6회 세척을 실시하여 pH 10.0∼11.0 범위로 맞춘다.443 ml of sodium hydroxide solution (purity 33%) was added to 10 L of purified water to prepare an alkaline aqueous solution of pH 13.4. Here, 1.0 kg of dried fish scales having a water content of 14% were added while operating the stirrer, and the stirrer was continued for 36 hours. After the completion of the alkali treatment, the alkaline water is completely drained and then washed six times with 10 L of purified water for about 30 minutes to adjust the pH to a range of 10.0 to 11.0.
알칼리 처리가 끝난 어류비늘 1㎏이 담긴 pH 10이하로 된 10L 물에 염산 용액(순도35%) 100㎖을 넣어서 pH 1.8로 하여 교반기를 계속 가동시키면서 24시간 지속시킨다. 이러한 산 처리가 종료된 후 산 처리수를 완전히 Drain 시킨 다음 10L 씩의 정제수로 약 30분씩 5회 세척을 실시하여 pH 4.5∼5.5 범위로 맞춘다.100 ml of hydrochloric acid solution (35% purity) was added to 10 L of water having a pH of 10 or less containing 1 kg of alkali-treated fish scales, and the pH was maintained at pH 1.8 and the stirrer was continued for 24 hours. After the acid treatment is completed, the acid treated water is completely drained, and then washed 5 times with 10 L of purified water for about 30 minutes to adjust the pH to 4.5 to 5.5.
원료의 전처리가 완료된 이러한 어류비늘을 50℃ 정제수 3L를 담은 추출용기에 넣는다. 추출용기 내의 용액의 pH는 5.0∼6.5범위를 유지하고, 추출용기 바닥에 설치된 스팀코일로 스팀을 공급하면서 용액을 펌프를 이용 자체 순환시킴으로써 용액의 온도를 45∼55℃로 유지시킨다. 추출시간을 8시간으로 추출된 용액의 젤라틴 농도는 6% 정도이며, 195g 상당의 젤라틴을 함유한다.The fish scales after the pretreatment of the raw material is completed are placed in an extraction container containing 3 liters of purified water 50 ℃. The pH of the solution in the extraction vessel is maintained in the range of 5.0 to 6.5, and the temperature of the solution is maintained at 45 to 55 ℃ by self-circulating the solution using a pump while supplying steam to the steam coil installed at the bottom of the extraction vessel. The extraction time is 8 hours, the gelatin concentration of the extracted solution is about 6%, and contains 195 g of gelatin.
추출된 용액을 받은 후 수산화나트륨(순도 33%)을 먼저 투입하여 pH 7.0∼7.5 범위로 조절하고, pH 7.0∼8.0 범위 내에서 수산화나트륨 수용액(순도 33%)과 무수 호박산 11g을 동시에 투입하면서 20분간 교반하여 치환시킨다.After receiving the extracted solution, sodium hydroxide (purity 33%) was added first to adjust the pH to 7.0-7.5 range, and sodium hydroxide aqueous solution (purity 33%) and 11 g of anhydrous succinic acid were simultaneously added within pH 7.0-8.0. Stir for minutes and replace.
치환이 완료된 호박산 젤라틴 용액은 1차 여과를 실시한 후 깨끗한 액을 이온교환수지를 통과시켜 미네랄을 제거하며, 이온교환수지를 통과한 용액의 pH는 수산화나트륨 수용액을 이용하여 pH 5.5∼6.0으로 조절한다.After completion of the succinate gelatin solution, the primary filtration is performed to remove minerals by passing the clean solution through the ion exchange resin, and the pH of the solution passed through the ion exchange resin is adjusted to pH 5.5-6.0 using an aqueous sodium hydroxide solution. .
이온교환수지를 통과한 용액을 2단계 멤브레인을 통과시켜 6%용액을 12%까지 자연 농축시킨 다음 2차 여과를 실시한다.The solution passed through the ion exchange resin was passed through a two-stage membrane to naturally concentrate the 6% solution to 12%, followed by secondary filtration.
2차 여과까지 완료된 용액을 진공 하에서 농축하여 농도 30∼35%로 유지시킨 다음 최종 3차 카본 필터 여과를 실시함으로써 완전히 정제된 용액 조건을 갖추도록 한다. 그리고 살균 후 통상의 방법으로 냉각시켜 건조를 한다.The solution completed until the secondary filtration is concentrated under vacuum to maintain a concentration of 30-35% and then subjected to a final tertiary carbon filter filtration to ensure fully purified solution conditions. After sterilization, the mixture is cooled by a conventional method and dried.
이러한 모든 공정을 거쳐 제조된 젤라틴의 강도는 242Bloom, 점도 45mPs, 치환도 96%의 건조된 호박산 젤라틴 190g을 얻었다.The strength of the gelatin prepared through all these processes was 190g of dried succinate gelatin with 242Bloom, viscosity 45mPs, substitution 96%.
(실시예 2)(Example 2)
5.0Kg의 우피(Hide Splits)를 가로 세로 5*5cm로 자른 다음 실시예 1에서와 같은 방법으로 제조된 젤라틴 강도는 223Bloom, 점도 50mPs, 치환도 94%의 건조된 호박산 젤라틴 602g을 얻었다.5.0Kg of Hide Splits were cut to 5 * 5cm in width and length, and gelatin strength of 223Bloom, viscosity of 50mPs, and 94% of substitution rate of 602g of dried succinate gelatin was obtained in the same manner as in Example 1.
(실시예 3)(Example 3)
5.0Kg의 돈피(Pig Skin)을 가로 세로 5*5cm로 자른 다음 실시예 1에서와 같은 방법으로 제조된 젤라틴 강도는 230Bloom, 점도 47mPs, 치환도 95%의 건조된 호박산 젤라틴 650g을 얻었다.5.0 Kg of pig skin (Pig Skin) was cut to 5 * 5cm in width and then the gelatin strength prepared in the same manner as in Example 1 was 230Bloom, viscosity 47mPs, 650g of dried succinate gelatin with 95% substitution degree.
(실시예 4)(Example 4)
3Kg 건조된 소뼈(Ossein)를 실시예 1에서와 같은 방법으로 제조된 젤라틴 강도는 232Bloom, 점도 49mPs, 치환도 95%의 건조된 호박산 젤라틴 450g을 얻었다.Gelatin strength of 3 kg dried bovine bone (Ossein) was prepared in the same manner as in Example 1 to obtain 450 g of dried succinate gelatin with 232Bloom, viscosity 49mPs, 95% substitution degree.
본 발명은 우피(Hide Splits), 돈피(Pig Skin), 건조된 소뼈(Ossein), 어류로부터 알칼리 처리, 산 처리, 알칼리와 산 처리를 겸하는 3단계의 전처리 공정 후 추출된 젤라틴 용액에 무수 호박산을 치환시켜 고품질의 호박산 젤라틴을 생산할 수 있게 되었다.In the present invention, succinic anhydride is extracted from gelatin solution extracted after three stages of pretreatment including alkaline treatment, acid treatment, alkali and acid treatment from hide splits, pig skin, dried ossein and fish. Substitution made it possible to produce high quality succinate gelatin.
또한 이렇게 생산된 호박산 젤라틴을 이용하여 캡슐의 붕해 실험을 한 결과 도 1과 같이 호박산 젤라틴이 일반 젤라틴에 비해 붕해성이 우수하게 나타남을 확인할 수 있었다. 가로축은 젤라틴 시료의 제조 후 경과기간을 나타낸 것이고 세로축은 젤라틴이 완전히 붕해되는 시간을 나타낸 것이다. 제조 후 2개월 이상이 지난 경우 호박산 젤라틴 캡슐에 비해 일반 젤라틴 캡슐은 약 50% 이상의 붕해 시간 지연을 초래하였다.In addition, as a result of the disintegration experiment of the capsule using the succinate gelatin produced in this way, it was confirmed that succinate gelatin showed excellent disintegration property compared to the normal gelatin as shown in FIG. The horizontal axis shows the elapsed time after preparation of the gelatin sample and the vertical axis shows the time for the gelatin to disintegrate completely. More than two months after manufacture, compared to succinic gelatin capsules, the normal gelatin capsules resulted in a disintegration time delay of about 50% or more.
본 발명은 우피(Hide Splits), 돈피(Pig Skin), 건조된 소뼈(Ossein), 어류로부터 알칼리 처리, 산 처리, 알칼리와 산 처리를 겸하는 3단계의 전처리 공정 후 추출된 젤라틴 용액에 무수 호박산을 치환시켜 고품질의 호박산 젤라틴을 생산할 수 있게 되었다. In the present invention, succinic anhydride is extracted from gelatin solution extracted after three stages of pretreatment including alkaline treatment, acid treatment, alkali and acid treatment from hide splits, pig skin, dried ossein and fish. Substitution made it possible to produce high quality succinate gelatin.
도 1은 35℃, 75% RH 하의 가혹한 조건에서 일반 젤라틴과 호박산 젤라틴의 붕해도 차이를 비교한 도면이다.1 is a diagram comparing the disintegration difference between normal gelatin and succinate gelatin under harsh conditions at 35 ° C. and 75% RH.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011059277A2 (en) * | 2009-11-13 | 2011-05-19 | Jang Yeo-Jin | Preparation method of packaging material for ramen soup |
| KR101960301B1 (en) * | 2018-11-16 | 2019-03-20 | 김경림 | Gelatine manufacturing system with an ion exchange resin tower integrated with pulp filter apparatus |
| KR101960300B1 (en) | 2018-11-08 | 2019-03-20 | 김경림 | Gelatine manufacturing system using pulp filter apparatus |
| KR101964696B1 (en) | 2018-12-13 | 2019-04-02 | 김경림 | A gelatin manufacturing system equipped with a pretreatment device capable of position modification of raw materials |
| KR102008944B1 (en) | 2019-06-26 | 2019-08-08 | 김경림 | Collagen extraction apparatus capable of both pretreatment step and extraction step, and collagen extraction method using the same |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100841206B1 (en) * | 2007-03-08 | 2008-06-24 | 남세준 | Making method of collagen food using pig skin |
| CN101914210A (en) * | 2010-09-01 | 2010-12-15 | 北京华达杰瑞生物技术有限公司 | Preparation process of succinylated gelatin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011059277A2 (en) * | 2009-11-13 | 2011-05-19 | Jang Yeo-Jin | Preparation method of packaging material for ramen soup |
| WO2011059277A3 (en) * | 2009-11-13 | 2011-09-22 | Jang Yeo-Jin | Preparation method of packaging material for ramen soup |
| KR101960300B1 (en) | 2018-11-08 | 2019-03-20 | 김경림 | Gelatine manufacturing system using pulp filter apparatus |
| KR101960301B1 (en) * | 2018-11-16 | 2019-03-20 | 김경림 | Gelatine manufacturing system with an ion exchange resin tower integrated with pulp filter apparatus |
| KR101964696B1 (en) | 2018-12-13 | 2019-04-02 | 김경림 | A gelatin manufacturing system equipped with a pretreatment device capable of position modification of raw materials |
| KR102008944B1 (en) | 2019-06-26 | 2019-08-08 | 김경림 | Collagen extraction apparatus capable of both pretreatment step and extraction step, and collagen extraction method using the same |
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