KR0173429B1 - Process for preparation of pearl solution with physical, chemical and biochemical method - Google Patents
Process for preparation of pearl solution with physical, chemical and biochemical method Download PDFInfo
- Publication number
- KR0173429B1 KR0173429B1 KR1019960000873A KR19960000873A KR0173429B1 KR 0173429 B1 KR0173429 B1 KR 0173429B1 KR 1019960000873 A KR1019960000873 A KR 1019960000873A KR 19960000873 A KR19960000873 A KR 19960000873A KR 0173429 B1 KR0173429 B1 KR 0173429B1
- Authority
- KR
- South Korea
- Prior art keywords
- supernatant
- pearl
- precipitate
- solids
- water
- Prior art date
Links
- 239000000126 substance Substances 0.000 title claims abstract description 14
- 238000002306 biochemical method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 28
- 238000002360 preparation method Methods 0.000 title description 11
- 239000006228 supernatant Substances 0.000 claims abstract description 45
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 108091005804 Peptidases Proteins 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000004365 Protease Substances 0.000 claims abstract description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract description 3
- 239000000872 buffer Substances 0.000 claims abstract description 3
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 3
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- 239000011049 pearl Substances 0.000 claims description 52
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000013505 freshwater Substances 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000011050 natural pearl Substances 0.000 claims description 2
- 238000009360 aquaculture Methods 0.000 claims 1
- 244000144974 aquaculture Species 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract description 4
- 239000000376 reactant Substances 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 102000004169 proteins and genes Human genes 0.000 description 19
- 108090000623 proteins and genes Proteins 0.000 description 19
- 239000000243 solution Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 9
- 239000011575 calcium Substances 0.000 description 9
- 229910052791 calcium Inorganic materials 0.000 description 9
- 239000002253 acid Substances 0.000 description 6
- 108010006161 conchiolin Proteins 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 230000000144 pharmacologic effect Effects 0.000 description 5
- 239000003651 drinking water Substances 0.000 description 4
- 235000020188 drinking water Nutrition 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012460 protein solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 102000035195 Peptidases Human genes 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241000590428 Panacea Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000010984 cultured pearl Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003797 essential amino acid Substances 0.000 description 1
- 235000020776 essential amino acid Nutrition 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000007952 growth promoter Substances 0.000 description 1
- 230000003779 hair growth Effects 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229940100656 nasal solution Drugs 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- -1 organic acid calcium salt Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229940024999 proteolytic enzymes for treatment of wounds and ulcers Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000009759 skin aging Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/16—Inorganic salts, minerals or trace elements
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2200/00—Function of food ingredients
- A23V2200/02—Antioxidant
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Polymers & Plastics (AREA)
- Zoology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Food Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Inorganic Chemistry (AREA)
- Dermatology (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Peptides Or Proteins (AREA)
- Cosmetics (AREA)
Abstract
본 발명은 물리, 화학 및 생화학적 방법을 이용한 수용성 진주액의 제조방법에 관한 것으로, 좀 더 상세하게는 외피를 제거한 진주를 100∼200메쉬의 입자크기로 분쇄시킨후, 1 내지 4배의 물을 첨가하여 밀봉시킨 다음, 100 내지 125℃, 1 내지 1.5기압에서 15분이상 반응시키고, 상기 반응물을 상온에서 충분히 정치시켜 고형분을 침전시킨후, 제1상등액을 분리시키는 제 1단계; 상기 제 1단계의 침전된 고형분에 식용빙초산액을 첨가하여 이산화탄소가 발생되지 않을때까지 반응시킨 다음, 고형분을 침전시키고 제2상등액을 분리시키는 제2단계; 상기 제2단계의 침전된 고형물과 염산을 반응시켜 탄산칼슘을 제거하고 세정한 다음, 최종액의 pH를 중성으로 전환시켜 침전물을 얻는 단계; 상기 침전물을 탄산나트륨 완충용액으로 분산시킨후, 단백질분해효소를 첨가하여 반응시킨 다음, 염산으로 중화시켜 제3상등액을 분리시키는 제3단계; 및 상기 제1상등액, 제2상등액 및 제3상등액을 적당한 비율로 혼합시키는 단계로 이루어지는 물리, 화학 및 생화학적 방법을 이용한 수용성 진주액의 제조방법에 관한 것이다.The present invention relates to a method for producing a water-soluble pearl liquid using physical, chemical and biochemical methods, and more specifically, 1 to 4 times water after pulverizing the pearl with the outer shell removed to a particle size of 100 to 200 mesh. Adding and sealing, and then reacting at 100 to 125 ° C. and 1 to 1.5 atmospheres for at least 15 minutes, allowing the reactant to sufficiently stand at room temperature to precipitate solids, and then separating the first supernatant; A second step of adding an edible ice acetate to the precipitated solids of the first step until the carbon dioxide is not generated and then precipitating the solids and separating the second supernatant; Reacting the precipitated solids with hydrochloric acid in the second step to remove calcium carbonate and washing, and then converting the pH of the final solution to neutral to obtain a precipitate; Dispersing the precipitate with sodium carbonate buffer, reacting with addition of protease, and neutralizing with hydrochloric acid to separate the third supernatant; And it relates to a method for producing a water-soluble pearl solution using a physical, chemical and biochemical method comprising the step of mixing the first supernatant, the second supernatant and the third supernatant in an appropriate ratio.
Description
제1도는 본 발명의 제조방법을 개략적으로 도시한 공정도.1 is a process diagram schematically showing a manufacturing method of the present invention.
본 발명은 물리, 화학 및 생화학적 방법을 이용한 수용성 진주액의 제조방법에 관한 것으로, 좀 더 상세하게는 일종의 진주가루 또는 진주조개의 외피를 취하여 분말을 제조한 후, 이로부터 수용성 활성단백질 및 칼슘염을 포함한 진주액을 물리, 화학 및 생화학적 방법을 이용하여 활성단백질의 함량이 높은 진주액을 제조하는 방법에 관한 것이다.The present invention relates to a method for preparing a water-soluble pearl liquid using physical, chemical and biochemical methods, and more particularly, to prepare a powder by taking a shell of a kind of pearl powder or pearl clam, and then from the water-soluble active protein and calcium The present invention relates to a method for preparing a pearl solution having a high content of active protein using a pearl solution containing a salt using physical, chemical and biochemical methods.
진주는 진주조개류 내부에서 생성되는 고형물질로서 비중은 2,238∼2.750, 경도는 4, 성분은 94%의 탄산칼슘과 6%의 유기물로 이루어져 있다. 이중 유기물의 대부분은 골격성 단백질(albuminoid)로 알려진 콘치올린(conchiolin)이 차지하고 있다. 상기 콘치올린은 단량체의 경우 분자량이 687.14, 분자식이 C32H98N2O11인 물질로 진주내의 탄산칼슘을 서로 연결시키는 진주의 구조를 이루게하는 자연결합 물질이다.Pearl is a solid material produced inside pearl shells. It has a specific gravity of 2,238 ~ 2.750, hardness of 4, and consists of 94% calcium carbonate and 6% organic matter. Most of these organisms are occupied by conchiolin, known as albuminoids. In the case of the monomer, the molecular weight of the monomer is 687.14, the molecular formula of C 32 H 98 N 2 O 11 is a natural binding material to form a structure of pearls connecting calcium carbonate in pearls.
이러한 진주는 예로부터 만병통치약이라하여 한방에서 널리 사용되어 왔다. 진주의 성분가운데 약리작용을 나타내는 것은 크게 칼슘과 콘치올린으로 구분될 수 있다. 칼슘은 섭취할 경우 뼈를 강화하며 혈압을 낮추고 항암작용도 있다고 한다. 얼굴이나 몸에 바를 경우는 화상의 치료제 또는 발모촉진제로도 사용이 가능하다 한편 코치올린은 체내에 섭취될 경우 혈액 순환장애의 개선작용이 있으며 역시 피부노화 방지작용이 탁월한 것으로 알려져 있다. 일본 및 중국에서는 고온에서 소결한 진주분말을 판매하고 있는데, 이 경우는 칼슘의 약리작용만이 효력을 발휘하며, 콘치올린 성분은 모두 파괴되어 이로인한 약리작용의 도움을 기대할 수는 없다.These pearls have been widely used in herbal medicine since ancient times as panacea. Among the components of pearls, pharmacological action is largely divided into calcium and conchiolin. Calcium, when ingested, strengthens bones, lowers blood pressure, and has anti-cancer effects. When applied to the face or body, it can be used as a burn remedy or hair growth promoter. On the other hand, koolin has been known to be effective in improving blood circulation and in preventing skin aging. In Japan and China, pearl powders sintered at a high temperature are sold. In this case, only the pharmacological action of calcium is effective, and all the conchiolin components are destroyed, so the pharmacological action cannot be expected.
진주의 성분인 탄산칼슘과 진주단백질은 물에 녹기 어렵고 위장에서 조차 매우 조금밖에 녹지 않기 때문에 체내에서 흡수되기 어렵다. 즉, 진주에 포함된 칼슘과 콘치올린은 그 상태로는 체내에 흡수되기 어려워 상술한 우수한 약리작용에도 불구하고 원하는 효과를 얻기 어렵다. 이러한 약리작용을 극대화하기 위하여 진주내의 유용한 성분을 수용성 형태로 변환시키는 연구가 요구되는 실정이다.Calcium carbonate and pearl proteins, which are the components of pearls, are difficult to be absorbed by the body because they are difficult to dissolve in water and very little in the stomach. In other words, calcium and conchiolin contained in pearls are difficult to be absorbed into the body in that state, and despite the excellent pharmacological action described above, it is difficult to obtain a desired effect. In order to maximize such pharmacological action, studies on converting useful components in pearls into water-soluble forms are required.
수용성 진주액은 진주내의 탄산칼슘과 산성물질이 반응하여 생성된 유기산 칼슘염과 가수분해된 수용성 콘치올린 단백질등 일련의 처리과정으로 얻어지는 일종의 담황색의 액체이다. 이 액체의 유효성분은 수용성 칼슘염 및 콘치올린 단백질(여러 인체 필수 아미노산을 함유), 염기성 인산염 및 미량원소로서 용도로는 진주추출액을 함유한 화장수, 항염 및 피부보호작용이 있는 크림 및 연고, 콘치올린을 유효성분으로 하는 화장품, 산화 방지제, 건강식품의 원료로 사용할 수 있다.Aqueous nasal solution is a kind of pale yellow liquid obtained through a series of treatments such as organic acid calcium salt and hydrolyzed water soluble conchiolin protein produced by the reaction of calcium carbonate and acid in pearl. The active ingredient of this liquid is water-soluble calcium salt and conchiolin protein (containing several human essential amino acids), basic phosphate and trace elements, and lotion containing pearl extract, cream and ointment with anti-inflammatory and skin protection, conch It can be used as a raw material for cosmetics, antioxidants, and health foods that use oline as an active ingredient.
상기 진주액을 제조하는 방법으로는 불용성 단백질을 가수분해하는 방법에 따라 가열가압법(물리적 방법), 산가수분해법(화학적 방법)과 효소법(생화학적 방법)으로 구분된다.The method of preparing the mother liquor is classified into a heating press method (physical method), an acid hydrolysis method (chemical method) and an enzyme method (biochemical method) according to a method of hydrolyzing an insoluble protein.
상기 가열가압법은 물에 침지된 진주가루에 여분의 물을 첨가하고 밀봉하여 온도 100∼130℃, 압력 50∼159KPa, 반응시간 10∼30분으로 반응시켜 수용액에 녹아나오는 수용성 단백질을 탈색, 탈염하여 제조한다. 제조된 용액의 단위 부피당 수율은 높으나 생산되는 용액의 절대 부피가 작아 전체 생산성은 매우 낮다. 또한, 상기 산가수분해법은 진주분말에 진한 염산 또는 황산을 이용하여 진주분말내의 탄산염을 제거하고 세척한 후, 여과, 가수분해, 산의 제거, 탈색, 탈염 등의 과정을 거쳐 진주액을 얻는다. 이 방법은 가수분해 조건이 매우 극심하여 단백질의 변성이 심하고 반응후의 잔류하는 산을 제거하는 번거로움이 있다. 한편 효소를 이용한 가수분해법은 강산으로 탄산칼슘을 제거한 후 잔류하는 불용성물질을 단백질분해효소로 가수분해하는 방법으로 기존의 산에 의한 가수분해에 비해 반응조건이 온화하고 부대시설이 간단하며 수율도 화학적 방법과 비교하여 동등한 우수한 방법이다.In the heating and pressing method, extra water is added to the pearl powder immersed in water and sealed to react with a temperature of 100 to 130 ° C., a pressure of 50 to 159 KPa, and a reaction time of 10 to 30 minutes to decolorize and dehydrate the water-soluble protein dissolved in the aqueous solution. To prepare. The yield per unit volume of the prepared solution is high but the overall productivity is very low due to the small absolute volume of the solution produced. In addition, the acid hydrolysis method removes and washes carbonate in the pearl powder using concentrated hydrochloric acid or sulfuric acid in the pearl powder, and then obtains pearl liquid through filtration, hydrolysis, acid removal, decolorization, desalting, and the like. In this method, hydrolysis conditions are very severe, and protein denaturation is severe, and it is troublesome to remove residual acid after the reaction. On the other hand, the enzyme hydrolysis method is to remove calcium carbonate with strong acid and hydrolyze the remaining insoluble substance with proteolytic enzyme. The reaction conditions are milder than the conventional hydrolysis by acid, and the facilities are simple and the yield is chemical. It is an excellent method equivalent to the method.
지금까지 보고된 연구는 상술한 물리, 화학 및 생화학적 방법중에서 한 가지만을 선택하여 진주액을 제조하였으며, 전량 외국산(중국과 일본) 진주를 이용한 결과이므로 국내에서 구입가능한 진주를 이용한 공정의 조업에 직접 적용할 수 없는 상황이다.The research reported so far has produced only one of the above-mentioned physical, chemical and biochemical methods, and the pearl liquid was produced. This is not the case.
이러한 상황하에서 본 발명자들은 상술한 세가지 공정을 결합시켜 동량의 진주분말에서 높은 수율로 진주의 유효성분을 취하여 수용성물질로 제조하는 방법을 발견하였다. 또한, 국내에서 생산되는 진주를 이용해 산처리시나 가수분해시에 사용되는 용제의 규칙성을 확립하여 전체적인 공정의 균일성을 달성할 수 있었다.Under these circumstances, the present inventors have found a method of combining the three processes described above to obtain an active ingredient of pearl in high yield in the same amount of pearl powder to produce a water-soluble substance. In addition, the uniformity of the overall process was achieved by establishing the regularity of the solvent used during acid treatment or hydrolysis using domestically produced pearls.
따라서, 본 발명의 목적은 물리, 화학 및 생화학적 방법을 이용하여 활성단백질의 함량이 높은 수용성 진주액을 제조하는 방법을 제공하는데 있다.Accordingly, it is an object of the present invention to provide a method for preparing a water-soluble pearl solution having a high content of active protein using physical, chemical and biochemical methods.
상기 목적을 달성하기 위한 본 발명의 방법은 외피를 제거한 진주를 100∼200메쉬의 입자크기로 분쇄시킨후, 1 내지 4배의 물을 첨가하여 밀봉시킨 다음, 100 내지 125℃, 1내지 1.5기압에서 15분 이상 반응시키고, 상기 반응물을 상온에서 충분히 정치시켜 고형분을 침전시킨후, 제1상등액을 분리시키는 제1단계; 상기 제1단계의 침전된 고형분에 식용빙초산액을 첨가하여 이산화탄소가 발생되지 않을때까지 반응시킨 다음, 고형분을 침전시키고 제2상등액을 분리시키는 제2단계; 상기 제2단계의 침전된 고형물과 염산을 반응시켜 탄산칼슘을 제거하고 세정한 다음, 최종액의 pH를 중성으로 전환시켜 침전물을 얻는 단계; 상기 침전물을 탄산나트륨 완충용액으로 분산시킨후, 단백질분해효소를 첨가하여 반응시킨 다음, 염산으로 중화시켜 제3상등액을 분리시키는 제3단계; 및 상기 제1상등액, 제2상등액 및 제3상등액을 적당한 비율로 혼합시키는 단계로 이루어진다.The method of the present invention for achieving the above object is pulverized pearls from which the outer shell is removed to a particle size of 100 to 200 mesh, and then sealed by adding 1 to 4 times water, then 100 to 125 ℃, 1 to 1.5 atm Reacting for at least 15 minutes at room temperature, and allowing the reactant to sufficiently stand at room temperature to precipitate solids, and then separating the first supernatant; A second step of adding the edible ice acetate to the precipitated solids of the first step until the carbon dioxide is not generated, and then precipitating the solids and separating the second supernatant; Reacting the precipitated solids with hydrochloric acid in the second step to remove calcium carbonate and washing, and then converting the pH of the final solution to neutral to obtain a precipitate; Dispersing the precipitate with sodium carbonate buffer, reacting with addition of protease, and neutralizing with hydrochloric acid to separate the third supernatant; And mixing the first supernatant, the second supernatant and the third supernatant in an appropriate ratio.
이하 본 발명을 좀 더 구체적으로 살펴보면 다음과 같다.Looking at the present invention in more detail as follows.
본 발명에 따른 수용성 진주액을 제조하는 방법에 사용되는 진주는 인근 해역에서 양식되는 바다진주, 강에서 양식하는 민물진주 및/또는 자연산 진주를 사용할 수 있지만, 경제적인 면을 고려하여 양식 진주가 바람직하다.The pearls used in the method for producing a water-soluble pearl liquid according to the present invention may use sea pearls, freshwater pearls and / or natural pearls grown in nearby waters, but cultured pearls are preferable for economic reasons. Do.
상기 진주의 외피는 진주분말을 제조하기 전에 제거한다. 외피가 제거된 진주는 분쇄기를 이용하여 입자의 크기가 100∼200메쉬(mesh)가 될 때까지 분쇄한 다음, 상기 진주분말을 적당한 용기에 넣은 후 여기에 적당량의 물을 부어 진주가루에 물을 흡수시킨후, 여분의 물을 붇는다. 이때 물의 양은 진주분말 질량의 1 내지 4배, 바람직하기는 2내지 3배가 적당하다. 그 다음, 상기 용기를 멸균기(autoclave)에 넣어 일정온도까지 천천히 가열한다. 가열온도 및 시간은 100℃인 경우 30분이상, 125℃인 경우는 15분에서 30분 사이가 바람직하다. 이때 압력은 게이지압력으로 1 내지 1.5기압이 바람직하다. 반응이 끝난 용기는 상온에서 충분한 시간을 정치시킨 후, 상등액을 여과하여 황갈색의 액체(제 1상등액)을 얻는다. 상기 제1상등액은 그 자체만으로도 상술한 용도로 사용할 수 있다. 따라서, 상기 제1상등액을 사용할 경우는 액체를 끓여 살균한 후 0.2%의 안식향산을 첨가하여 적당한 용기에 담아 밀봉시켜 보관한다.The shell of the pearl is removed before the pearl powder is made. Pearls from which the outer shell is removed are ground using a grinder until the particle size becomes 100 to 200 mesh, and then, the pearl powder is placed in a suitable container, and then poured an appropriate amount of water into the pearl powder. After absorption, drain excess water. At this time, the amount of water is 1 to 4 times, preferably 2 to 3 times the mass of the pearl powder. The vessel is then heated in a sterilizer (autoclave) slowly to a certain temperature. The heating temperature and time is preferably 30 minutes or more at 100 ° C and 15 to 30 minutes at 125 ° C. At this time, the pressure is preferably 1 to 1.5 atm as the gauge pressure. After the reaction, the vessel is allowed to stand at room temperature for sufficient time, and then the supernatant is filtered to give a yellowish brown liquid (first supernatant). The first supernatant can be used for the above-mentioned purposes alone. Therefore, in the case of using the first supernatant, the liquid is boiled and sterilized, and 0.2% benzoic acid is added and sealed in a suitable container and stored.
그렇지 않을 경우는 다음 단계로 넘어간다.If not, go to the next step.
상술한 단계에서 상기 제1상등액을 제거시키고 잔존하는 침전된 진주분말에 5∼15%의 식용빙초산액을 천천히 첨가하면서 교반한다. 이때 반응온도는 60 내지 70℃사이가 바람직하다. 이산화탄소가 발생되지 않을 때를 반응이 끝난 시점으로 간주하여 상등액(제2상등액)을 회수한다. 상기 제2상등액은 초산칼슘염을 포함하는 황갈색의 투명한 액체이다. 첨가하는 초산의 농도에 따라 전체 첨가되는 부피가 결정된다.In the above-described step, the first supernatant is removed and stirred while slowly adding 5-15% of an edible ice acetic acid solution to the remaining precipitated pearl powder. At this time, the reaction temperature is preferably between 60 and 70 ℃. When no carbon dioxide is generated, the supernatant (second supernatant) is recovered. The second supernatant is a yellowish brown transparent liquid containing calcium acetate salt. The total volume added depends on the concentration of acetic acid added.
초산반응 후, 침전된 물질에 1노르말(Normal)농도의 염산을 무게비로 1:1로 서서히 첨가하면서 미반응된 탄산칼슘을 제거한다. 반응조건은 초산을 이용한 반응과 동일하다. 약 3시간정도 반응한 후 상등액을 제거하고, 침전물은 식용수로 여러차례 세정하여 최종액의 pH가 중성이 되도록 한다. 세정이 끝난 침전물은 여과하여 흑갈색의 불용성 단백질 분말을 얻는다.After the acetic acid reaction, unreacted calcium carbonate is removed by slowly adding 1: 1 normal concentration of hydrochloric acid at a weight ratio of 1: 1 to the precipitated material. The reaction conditions are the same as the reaction using acetic acid. After reacting for about 3 hours, the supernatant is removed and the precipitate is washed several times with drinking water so that the pH of the final solution is neutral. The washed precipitate is filtered to give a dark brown insoluble protein powder.
상기 불용성단백질을 다른 용기에 이동시킨후, 탄산나트륨 완충용액(pH 10∼12)에 분산시킨다. 분산된 용액에 상용화되있는 단백질 가수분해효소를 상기 불용성단백질에 대하여 적어도 0.001중량% 이상 첨가한 후, 30 내지 50℃의 반응온도에서 교반하면서 1 내지 24시간 반응시킨다. 반응이 끝난 용액은 여과하여 침전물은 폐기하고 상등액은 6노르말 염산을 이용하여 중성의 pH로 조절하다. 이 용액을 가열하여 멸균한 후 여과하여 최종 수용성 단백질액(제3상등액)을 얻는다.The insoluble protein is transferred to another vessel and then dispersed in sodium carbonate buffer solution (pH 10-12). Proteolytic enzymes that are compatible with the dispersed solution are added to the insoluble protein at least 0.001% by weight or more, and then reacted for 1 to 24 hours with stirring at a reaction temperature of 30 to 50 ° C. The reaction solution is filtered and the precipitate is discarded. The supernatant is adjusted to neutral pH using 6-normal hydrochloric acid. The solution is heated to sterilize and then filtered to obtain a final water soluble protein solution (third supernatant).
상술한 제1상등액, 제2상등액 및 제3상등액을 적당한 비율, 바람직하게는 1:1:1의 비율로 혼합하여 칼슘농도 500∼5000ppm, 단백질농도 0.5∼1.0mg/mL의 본 발명의 수용성진주액을 제조한다.The water-soluble pearl of the present invention having a calcium concentration of 500-5000 ppm and a protein concentration of 0.5-1.0 mg / mL by mixing the first supernatant, the second supernatant, and the third supernatant in an appropriate ratio, preferably in a ratio of 1: 1: 1. Prepare a liquid.
진주액내에 포함된 칼슘의 농도는 원자흡광분석방법(AAS)으로, 단백질의 농도는 미국 시그마(Sigma Co.)사에서 제공하는 BCA(BiCinconinic acid) 키트를 이용하여 측정하였다.The concentration of calcium contained in the nacre was measured by atomic absorption spectrometry (AAS), and the protein concentration was measured using a BiCinconinic acid (BCA) kit provided by Sigma Co., Ltd., USA.
이하 제조예 및 실시예를 통하여 본 발명을 좀 더 구체적으로 설명하지만, 하기 예에 본 발명의 범주가 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Preparation Examples and Examples, but the scope of the present invention is not limited to the following Examples.
[제조예 1][Production Example 1]
[고온고압법(제1상등액의 제조)][High temperature high pressure method (production of the first supernatant)]
양식 바다진주 10g과 양식 민물진주 10g을 각각 2개의 별도의 용기에 담아 식용수를 각 진주시료 별로 20밀리리터와 30밀리리터를 첨가한 후(총 4개의 시료), 125℃에서 15분간 반응시켰다. 생성된 액체를 상온에서 하루동안 정치시킨 후 상등액을 여과하여 제1상등액을 얻는다. 이렇게 얻어진 상기 제1상등액의 단백질 농도는 바다진주가 1.4mg/mL(총 부피 30밀리리터)와 2.8mg/mL(총 부피 20밀리리터)이였으며, 민물진주는 1.2mg/mL(총 부피 30밀리리터)및 2.5mg/m L(총 부피 20밀리리터)이였다. 본 제조예에서 첨가하는 물의 양을 조절하면 더욱 농축된 진주농축액을 제조할 수 있다. 또한, 반응조건은 100℃에서 30분 또는 80℃에서 3시간 반응시키는 것으로 대치할 수 있다.Ten grams of cultured sea pearls and 10 grams of freshwater pearls were placed in two separate containers, and 20 ml and 30 ml of drinking water was added to each pearl sample (four samples in total), followed by reaction at 125 ° C. for 15 minutes. The resulting liquid is allowed to stand at room temperature for one day, and then the supernatant is filtered to obtain a first supernatant. The protein concentrations of the first supernatant thus obtained were 1.4 mg / mL (30 milliliters total volume) and 2.8 mg / mL (20 milliliters total volume) of sea pearls, and 1.2 mg / mL (30 milliliters total volume) of fresh water pearls. And 2.5 mg / m L (total volume 20 milliliters). By adjusting the amount of water added in the present preparation can be prepared more concentrated pearl concentrate. In addition, reaction conditions can be replaced by making it react at 100 degreeC for 30 minutes or 80 degreeC for 3 hours.
[제조예 2][Production Example 2]
[화학적 방법(제2상등액의 제조)][Chemical Method (Preparation of Second Supernatant)]
상기 제조예 1에서 얻은 침전물 50g에 7% 식용빙초산 800밀리리터를 천천히 첨가한다. 이때 교반은 소형 교반기를 이용하였으며 반응온도는 60℃였다. 황색의 뿌연 액체가 생성되면 이것을 상온까지 냉각하여 진주초산염(액체)과 나머지 불용성 물질(고체)를 얻는다. 3시간 반응하여 750밀리리터의 황갈색의 액체(제2상등액)를 여과하여 얻었다. 상기 제2상등액에는 12,000ppm의 칼슘과 0.5mg/mL의 단백질의 함유되어 있다. 생성된 10g의 불용성물질을 다른 용기에 담은 후, 1노르말의 염산 100밀리리터를 넣어 충분히 교반한 후 상등액을 제거시킨 다음, 적당량의 식용수를 부어 세정작업을 반복하여 식용수의 pH가 중성일 때까지 이 공정을 반복한다. 최종적으로 진공건조하여 1.2g의 불용성 단백질을 얻었다.To 50 g of the precipitate obtained in Preparation Example 1, 800 ml of 7% edible glacial acetic acid was slowly added. At this time, the stirring was performed using a small stirrer and the reaction temperature was 60 ℃. When a yellow cloudy liquid is produced, it is cooled to room temperature to obtain pearl acetate (liquid) and the remaining insoluble matter (solid). After reacting for 3 hours, 750 milliliters of a yellowish brown liquid (second supernatant) was obtained by filtration. The second supernatant contains 12,000 ppm calcium and 0.5 mg / mL protein. Put 10g of insoluble substance produced in another container, add 100 ml of 1 normal hydrochloric acid, stir it sufficiently, remove the supernatant, and pour the appropriate amount of drinking water and repeat the washing process to make the pH of drinking water neutral. Repeat this process until. Finally, vacuum drying yielded 1.2 g of insoluble protein.
[제조예 3][Manufacture example 3]
[생화학적 방법(제3상등액의 제조)]Biochemical Method (Preparation of Third Supernatant)
상기 제조예 2에서 얻은 불용성 단백질을 300밀리리터의 Na2Co`용액에 분산시킨 후, 1N의 가성소다용액을 이용하여 pH를 10.5로 조정한다. 반응온도는 35℃, 효소는 솔베이사의 OPTIMASE를 5밀리리터 첨가하여 15시간 반응하였다. 가용화된 액은 1N염산을 이용해 pH를 중성으로 서서히 떨어뜨리고, 이 액은 여과하여 고형물은 분리한다. 최종적으로 1.5mg/mL의 단백질 농도의 제3상등액 350밀리리터를 얻었다.The insoluble protein obtained in Preparation Example 2 was dispersed in 300 ml of Na 2 Co ` solution, and then the pH was adjusted to 10.5 using 1N caustic soda solution. The reaction temperature was 35 ° C, and the enzyme was reacted for 15 hours by adding 5 milliliters of Solvay's OPTIMASE. The solubilized solution is gradually lowered to neutral with 1N hydrochloric acid, and the solution is filtered to separate the solids. Finally, 350 milliliters of the third supernatant with a protein concentration of 1.5 mg / mL was obtained.
[실시예 1]Example 1
[진주초산염과 단백질을 함유한 진주액의 제조][Preparation of Pearl Juice Containing Pearl Acetate and Protein]
상기 제조예 1에서 얻은 단백질용액, 제조예 2에서 얻은 칼슘염 용액 및 제조예 3에서 얻은 단백질용액을 1:1:1의 비율로 혼합하여 칼슘의 농도가 4000ppm이고 단백질의 농도가 1.3mg/mL인 진주액을 제조하였다.The protein solution obtained in Preparation Example 1, the calcium salt solution obtained in Preparation Example 2 and the protein solution obtained in Preparation Example 3 were mixed in a ratio of 1: 1: 1, and the calcium concentration was 4000 ppm and the protein concentration was 1.3 mg / mL. Phosphorus pearl solution was prepared.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019960000873A KR0173429B1 (en) | 1996-01-17 | 1996-01-17 | Process for preparation of pearl solution with physical, chemical and biochemical method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019960000873A KR0173429B1 (en) | 1996-01-17 | 1996-01-17 | Process for preparation of pearl solution with physical, chemical and biochemical method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR970058715A KR970058715A (en) | 1997-08-12 |
| KR0173429B1 true KR0173429B1 (en) | 1999-02-01 |
Family
ID=19449592
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1019960000873A KR0173429B1 (en) | 1996-01-17 | 1996-01-17 | Process for preparation of pearl solution with physical, chemical and biochemical method |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR0173429B1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040006092A (en) * | 2002-07-09 | 2004-01-24 | 서숙 | Dermis-accelerant Including the Fine Pure Pearl Powder |
| KR100549399B1 (en) * | 2002-07-09 | 2006-02-03 | (주) 진주본 | The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature |
| KR101313266B1 (en) * | 2010-10-11 | 2013-09-30 | 양승필 | High-calcium soybean curd containing pearl material and Making method thereof |
| KR20160135743A (en) * | 2014-03-14 | 2016-11-28 | 오스문 바이오로지컬 씨오.,엘티디. | Method for separating and preparing pearl extract from pearls |
| KR20210054679A (en) * | 2019-11-06 | 2021-05-14 | 안은영 | Manufacturing method of food, health functional food and cosmetic composition using water-soluble pearl capsule |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100397682B1 (en) * | 2001-02-26 | 2003-09-13 | 송선자 | Ionized calcium and ionized calcium water made of pearl shell and preparation method of the same |
-
1996
- 1996-01-17 KR KR1019960000873A patent/KR0173429B1/en not_active IP Right Cessation
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040006092A (en) * | 2002-07-09 | 2004-01-24 | 서숙 | Dermis-accelerant Including the Fine Pure Pearl Powder |
| KR100549399B1 (en) * | 2002-07-09 | 2006-02-03 | (주) 진주본 | The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature |
| KR101313266B1 (en) * | 2010-10-11 | 2013-09-30 | 양승필 | High-calcium soybean curd containing pearl material and Making method thereof |
| KR20160135743A (en) * | 2014-03-14 | 2016-11-28 | 오스문 바이오로지컬 씨오.,엘티디. | Method for separating and preparing pearl extract from pearls |
| KR20210054679A (en) * | 2019-11-06 | 2021-05-14 | 안은영 | Manufacturing method of food, health functional food and cosmetic composition using water-soluble pearl capsule |
Also Published As
| Publication number | Publication date |
|---|---|
| KR970058715A (en) | 1997-08-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103843970B (en) | Production method for preparing ossein oligopeptide meal, bone oil and bone meal | |
| TWI516280B (en) | Use of chenopodium formosanum extract for manufacture of composition for enhancing secretion of collagen and preventing cutaneous aging | |
| CN107751697A (en) | Chlorella extract phycocyanin drink with function preparation method | |
| CN105341933A (en) | Trepang and oyster enzymolysis oral liquid and preparation method thereof | |
| CN104041831A (en) | Soft peony peptide capsule and preparation method thereof | |
| KR0173429B1 (en) | Process for preparation of pearl solution with physical, chemical and biochemical method | |
| CN101965897A (en) | Processing method for mussel isolated protein | |
| CN109504722A (en) | A kind of method that amylorrhexis prepares chitosan oligosaccharide chelated selenium | |
| KR100549399B1 (en) | The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature | |
| JPH06135848A (en) | Active oxygen scavenger composition | |
| CN107836613A (en) | Chlorella growth factor spirulina polysaccharide drink with function preparation method | |
| KR20110031669A (en) | Process for fiber drinks using a sea-slug and fiber drinks thereof | |
| KR100876921B1 (en) | Method for tenderizing shell of crustacean or animal horny substance | |
| CN111820406A (en) | Polypeptide resveratrol preparation, preparation method and application thereof, and health-care product or pharmaceutical composition containing polypeptide resveratrol preparation | |
| CN106692257B (en) | A kind of combination of pectins, preparation method and its usage | |
| KR20010070692A (en) | Development of functional foods on improvement of immune system and antioxidant in utilization of Canavalia glaviata | |
| KR100397682B1 (en) | Ionized calcium and ionized calcium water made of pearl shell and preparation method of the same | |
| CN104862364B (en) | Bee pollen form cole Oligopeptide Compositions and preparation method thereof | |
| SU1081843A1 (en) | Method of producing protein hydrolysate from sunflower grist | |
| KR20010085034A (en) | Process for preparing calcium supplement from starfish | |
| JP7423803B2 (en) | Process method for efficiently producing carnosine-rich compounds | |
| JPH01273560A (en) | Hem iron solution or beverage containing the same solution | |
| CN114317656B (en) | Bioactive hairtail peptide microelement chelate and preparation method thereof | |
| CN1082349C (en) | Edible tree fungi extracting liquid containing amino acids and its application | |
| CN106868074A (en) | A kind of high activity peanut chitin and preparation method thereof |
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 | ||
| FPAY | Annual fee payment |
Payment date: 20041101 Year of fee payment: 7 |
|
| LAPS | Lapse due to unpaid annual fee |