KR20020065433A - The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature - Google Patents

The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature Download PDF

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KR20020065433A
KR20020065433A KR1020020039752A KR20020039752A KR20020065433A KR 20020065433 A KR20020065433 A KR 20020065433A KR 1020020039752 A KR1020020039752 A KR 1020020039752A KR 20020039752 A KR20020039752 A KR 20020039752A KR 20020065433 A KR20020065433 A KR 20020065433A
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water
acid
pearl
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pearl powder
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원종찬
조문구
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주식회사 진주나라
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/6261Milling

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Abstract

PURPOSE: A water soluble pearl powder using acid hydrolysis in normal temperature is provided, which has improved absorption of calcium into human body and fortifies immune system. CONSTITUTION: The preparation method of water soluble pearl powder includes the steps of pulverizing pearl into 500 to 1000 mesh size; adding two or three times of water to the pearl powder followed by filtering; reacting 1-20 vol.% of glacial acetic acid with solids obtained in a second step at 350 to 600 rpm until CO2 gas is not generated any more; filtering above solution to separate solid fraction from liquid fraction; rinsing the solid fraction with distilled water to remove residual aqueous soluble components; spray drying liquid fraction to prepare water soluble pearl calcium and protein powder; and mixing obtained pearl powder with mushroom extracts, silk amino acid, and vitamin D.

Description

상온 산가수분해법을 이용한 수용성 진주분말의 제조방법{The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature}The method of preparing water-soluble pearl powder using acid hydrolysis in normal temperature}

본 발명은 상온 산가수분해법을 이용한 수용성 진주칼슘의 제조방법에 관한 것으로서, 더욱 상세하게는 진주의 탄산칼슘과 산성물질이 반응하여 생성된 칼슘염과 미량의 가수분해된 수용성 단백질 등 일련의 처리과정에서 얻어지는 일종의 순백색-미백색의 분말로 이 분말의 유효성분은 수용성 칼슘염, 콘키올린 단백질(여러 가지 필수아미노산 함유), 미량원소로 화장품, 항염 및 피부보호작용이 있는 크림과 연고, 건강식품 및 각종 식품의 첨가 원료로 사용할 수 있는 수용성 진주분말의 제조방법에 관한 것이다.The present invention relates to a method for preparing water-soluble pearl calcium using room temperature acid hydrolysis, and more particularly, to a series of treatment processes such as calcium salt produced by the reaction of calcium carbonate and an acidic substance of pearl and a small amount of hydrolyzed water-soluble protein. It is a kind of pure white-white powder obtained from. Its active ingredient is water-soluble calcium salt, conchiolin protein (containing several essential amino acids), trace elements as cosmetics, creams and ointments with anti-inflammatory and skin protection, health food and various The present invention relates to a method for producing a water-soluble pearl powder that can be used as a raw material for adding food.

일반적으로, 진주는 진주조개류 내부에서 생성되는 고형물질이며, 주요성분은 CaCo391.7%의 탄산칼슘과 5.7%의 기타유기물, 수분 2.2%로 이루어져 있다.유기물은 대부분이 골격성 단백질로 알려진 콘키올린(conchiolin)이 차지하고 있다. 콘키올린은 7 ∼ 14종의 아미노산으로 이루어진 천연단백질로서 진주의 주성분인 탄산칼슘을 서로 결합하여 진주의 형태를 형성시키는 자연결합성 물질이다.In general, pearls are a solid substance produced in the shellfish, and the main component is CaCo 3 91.7% calcium carbonate, 5.7% other organic matter and 2.2% moisture. (conchiolin) occupies. Conchiolin is a natural protein consisting of 7 to 14 amino acids and is a natural binding substance that forms calcium in the form of pearls by binding calcium carbonate, which is a major component of pearls, to each other.

또한, 진주는 고대로 한방 약재로 사용되어져 왔으며, 한의학대사전에 의하면 "진주는 맛은 달고 짜며 성질은 차다. 정신을 안정시키고 경련을 진정시키며 가래를 삭이고 간열을 없애며 눈을 밝게 한다. 또한 새살이 돋아나게 하고 헌데를 잘 아물게 한다. 소아경풍(驚風), 심계항진, 수면장애, 이롱(耳聾), 소갈병(消渴病), 간열(肝熱)로 눈이 충혈되면서 시큰 거리는데 효과가 좋다."라고 쓰여져 있다. 이렇듯 민간약재로 다양하게 쓰여져 오던 진주의 성분은 생리활성을 나타내는 칼슘과 콘키올린이며, 이 외에 소량이 함유되어 있는 무기성분들이다. 칼슘은 섭취할 경우 뼈를 강화하며 혈압을 낮추고 소화촉진 및 건위작용도 있다고 한다. 얼굴과 피부에 바를 경우는 화상의 치료제 또는 발모촉진제로도 사용이 가능하다.In addition, pearls have been used as an herbal medicine in ancient times, and according to the Korean Medicine Dictionary, "Pearls are sweet, salty, and cold. And boils well. Pediatric sensation (驚風), palpitations, sleep disorders, yilong (耳聾), small brown disease (간), liver fever, and redness of the eyes are good to tingle. " It is written. As such, pearls, which have been used in various folk medicines, are calcium and conchiolin which exhibit physiological activities, and inorganic ingredients that contain small amounts. Calcium, when ingested, strengthens bones, lowers blood pressure, promotes digestion, and is also said to be healthy. When applied to face and skin, it can also be used as a burn remedy or hair growth promoter.

상기, 콘키올린은 아미노산 복합물질로서 섭취할 경우 혈액순환장애의 개선작용이 있으며 피부노화 방지작용도 우수한 것으로 알려져 있다. 일본과 중국에서는 고온에서 소결 가공한 진주분말이 상품화되어 있으나, 이 경우는 진주의 활성 성분중에서 칼슘과 무기성분만이 효력을 발휘하며 단백질성분은 모두 소실되고, 회분의 증가로 인해 약리작용의 도움을 기대할 수 없다.The conchiolin is known to have an effect of improving blood circulation disorders and to prevent skin aging when ingested as an amino acid complex. In Japan and China, pearl powders sintered at high temperatures are commercialized, but in this case, only calcium and inorganic components are effective among the active ingredients of pearls, and all protein components are lost. Can not expect

진주는 오염되지 않은 천연의 조건에서만 양식되어지는 고칼슘으로, 중금속 오염등의 염려가 되는 패각칼슘과 광우병의 우려가 있는 우골분등 안전성에 의심이 되는 여타의 칼슘제품과 차별화 될 수 있으나, 체내 흡수율에 문제가 되었던 것이사실이다.Pearl is a high calcium cultured only in uncontaminated natural conditions, and can be differentiated from other calcium products that are suspected of safety, such as shell calcium, which may cause heavy metal contamination, and cow bone powder, which may cause mad cow disease. It was a matter of fact.

종래의 수용성 진주분말을 제조하는 방법은 진주의 주성분인 탄산칼슘과 불용성 단백질 성분을 가수분해하는 방법에 따라 물리적(가열가압법), 화학적(산알카리법)과 생화학적(효소법) 방법으로 구분된다.Conventional methods for preparing water-soluble pearl powders are classified into physical (heating) method, chemical (acid alkali method) and biochemical (enzyme method) according to methods of hydrolyzing calcium carbonate and insoluble protein components, which are the main components of pearls. .

제조예 1. 물리적 방법(가열가압법)Preparation Example 1 Physical Method (Heating Press Method)

진주분말을 수용액에 가하고 밀폐시켜 온도 90 ∼ 150, 압력 50 ∼ 150kPa에서 10분 ∼ 1시간 동안 반응시켜 수용액에 용출되는 수용성 단백질을 탈색 및 탈염시킨 것을 건조하여 제조한다. 반응시키는 수용액의 단위부피당 수율은 높지만 처리하는 수용액의 절대부피가 작아 전체생산성은 매우 낮다.The pearl powder is added to an aqueous solution, sealed, and reacted for 10 minutes to 1 hour at a temperature of 90 to 150 and a pressure of 50 to 150 kPa to decolorize and dehydrate the water-soluble protein eluted in the aqueous solution. Although the yield per unit volume of the aqueous solution to react is high, the absolute volume of the aqueous solution to be treated is small, so that the overall productivity is very low.

제조예 2. 화학적 방법(산알카리 가수분해법)Preparation Example 2 Chemical Method (Acid Alkaline Hydrolysis)

진주분말에 진한 산이나 묽은 알카리 수용액을 첨가하여 탄산염을 제거하고 세척여과, 가수분해, 중화, 탈색, 탈염 등의 과정을 거치거나, 묽은 알카리와 알콜수용액에서 단백질성분을 가수분해, 중화, 여과 등의 과정을 거쳐야 한다.Remove the carbonate by adding concentrated acid or dilute alkaline aqueous solution to the pearl powder, and then wash filtration, hydrolysis, neutralization, decolorization, desalting, or hydrolyze, neutralize, and filter protein components in dilute alkaline and alcoholic solutions. You must go through the process.

제조예 3. 생화학적 방법(효소법)Preparation Example 3 Biochemical Method (Enzyme Method)

탄산칼슘을 제거하고 잔류한 불용성물질을 단백질 가수분해효소와 반응시켜 수용액으로 용출시키고, 효소를 불활성화 시킨 다음 여과 건조한다. 다른 방법에 비하여 반응조건이 온화하며 부대시설이 간단하고 수율이 화학적 방법과 대등하지만 효소의 가격이 비싸고, 완벽한 가수분해가 어렵다. 또한 반응이 완료된 다음 잔류하는 효소단백으로 인한 수용액의 탁도 증가 등의 문제가 있다.Calcium carbonate is removed and the remaining insoluble matter is reacted with proteolytic enzymes to elute it with an aqueous solution. The enzyme is inactivated and then filtered and dried. Compared with other methods, the reaction conditions are milder, the auxiliary facilities are simpler, and the yields are comparable with chemical methods, but the enzyme is expensive and the complete hydrolysis is difficult. In addition, there is a problem such as increased turbidity of the aqueous solution due to the remaining enzyme protein after the reaction is completed.

상기의 제조예로 제조되어진 진주분말에 있어, 진주의 주성분인 탄산칼슘과단백질은 물에 거의 녹지 않으며 위장관에서도 매우 적은 양만이 녹기 때문에 체내에서 흡수되기가 어렵다.In the pearl powder prepared by the above preparation, calcium carbonate and protein, which are the main components of pearl, are hardly soluble in water and are difficult to be absorbed in the body because only a very small amount is dissolved in the gastrointestinal tract.

즉, 진주에 함유된 칼슘과 단백질은 원래상태로는 체내에 흡수가 어려워 상술한 우수한 생리활성에도 불구하고 원하는 효과를 얻기가 어렵다. 이러한 생리활성을 극대화시키기 위하여 진주의 유용성분을 수용성으로 전환시켜 체내흡수를 쉽게 하려는 시도가 이루어지고 있다.That is, calcium and protein contained in pearls are difficult to be absorbed into the body in the original state, and thus, despite the excellent physiological activity described above, it is difficult to obtain a desired effect. In order to maximize such physiological activity, attempts have been made to easily convert the useful components of pearls into water-soluble and absorb the body.

지금까지 보고된 연구결과들은 상술한 물리, 화학 및 생화학적 방법 중에서 한 가지 또는 2가지 이상을 선택하여 수용성 진주분말을 제조하였으나, 과다한 에너지사용, 복잡한 처리공정, 처리비용과 낮은 효율로 상업화에 직접 적용하기가 어려운 상황이다.The research results reported so far have produced water-soluble pearl powder by selecting one or two or more of the above-mentioned physical, chemical and biochemical methods. It is a difficult situation to apply.

본 발명은 상술한 공정의 문제점인 에너지 사용량을 획기적으로 감소시키고 동량의 진주분말에서 높은 수율로 진주의 유효성분을 취하여 수용성물질로 제조하는 방법을 개발하였다. 또한, 산가수분해 과정에 사용하는 용제의 규칙성을 확립하여 전체적인 공정의 균일성을 달성할 수 있도록 한 것이다.The present invention has been developed a method for producing a water-soluble material by dramatically reducing the energy consumption, a problem of the above-described process and taking the active ingredient of pearl in high yield in the same amount of pearl powder. In addition, the regularity of the solvent used in the acid hydrolysis process is established to achieve the uniformity of the overall process.

따라서 본 발명의 목적은 물리적 및 화학적 방법을 이용하여 칼슘과 활성단백질의 함량이 높은 수용성 진주분말의 제조방법을 제공하며, 버섯다당체추출물, 뮤코다당단백, 실크아미노산, 비타민 D 등을 혼합하여 체내 칼슘흡수율을 높이고 면역강화와 피부노화방지를 유도할 수 있는 기능성의 수용성진주분말을 제조하는데있다.Accordingly, an object of the present invention is to provide a method for preparing a water-soluble pearl powder having a high content of calcium and active protein by using physical and chemical methods, by mixing mushroom polysaccharide extract, mucopolysaccharide protein, silk amino acid, vitamin D, etc. It is to manufacture functional water-soluble pearl powder that can increase absorption rate and induce immunity enhancement and skin aging prevention.

상기 목적을 달성하기 위한 본 발명의 방법은 진주를 500 ∼ 1,000메쉬의 입자크기로 분쇄한 다음 5 ∼ 20%(v/v)식용 빙초산 수용액을 첨가하여 이산화탄소가 발생되지 않을 때까지 350 ∼ 600rpm, 상온에서 반응시키고, 교반을 중지하고 고형분을 침전시켜 제1액을 분리시키는 제 1 단계; 상기, 제 1 단계의 고형분과 동일한 부피의 정제수를 가해 2 ∼ 3회 잔류성분과 불용성 고형분을 분리하는 제 2 단계; 상기 제1액과 제2액을 혼합하여 중화 또는 여과하고 분무 건조하여 수용성 진주칼슘을 제조하는 제 3 단계; 수용성 진주칼슘을 그대로 또는 버섯다당체추출물, 뮤코다당단백, 실크아미노산, 비타민 D 등을 혼합하여 기능성의 수용성 진주분말을 제조하는 단계로 이루어진다.The method of the present invention for achieving the above object is pulverized pearl to 500 ~ 1,000 mesh particle size and then added to 5 ~ 20% (v / v) aqueous solution of edible glacial acetic acid 350 ~ 600rpm, until no carbon dioxide is generated, A first step of reacting at room temperature, stopping stirring and precipitating solids to separate the first liquid; A second step of separating residual components and insoluble solids two or three times by adding purified water having the same volume as the solids of the first step; A third step of mixing the first liquid and the second liquid to neutralize or filter and spray-dry to prepare a water-soluble pearl calcium; Soluble pearl calcium as it is or mixed with a mushroom polysaccharide extract, mucopolysaccharide protein, silk amino acid, vitamin D and the like is made to prepare a functional water-soluble pearl powder.

본 발명에 따른 수용성 진주칼슘을 제조하는 방법에 사용하는 진주는 국내 양식산업의 미비함으로 인해 경제성을 고려하여 중국이나 인도네시아 연안해역에서 양식되는 바다진주, 강에서 양식하는 민물진주 및 자연산 진주 중에서 상품가치가 없는 등외품을 이용하는 것이 바람직하다.Pearls used in the method for producing water-soluble pearl calcium according to the present invention has a commodity value among sea pearls, freshwater pearls and natural pearls grown in the Chinese or Indonesian coastal waters due to their lack of domestic aquaculture. It is preferable to use an external product without the like.

상기, 진주를 분쇄기에서 입자의 크기가 500 ∼ 1,000메쉬가 될 때까지 분쇄한 다음 적당한 용기에 넣고 적당량의 물을 가해 진주가루에 물을 흡수시킨 후 여분의 물을 가한다. 이때 1 ∼ 2회 세척여과를 실시한다.The pearls are pulverized in a pulverizer until the particle size is 500 to 1,000 mesh, and then put in a suitable container, an appropriate amount of water is added to absorb pearl water, and then extra water is added. At this time, wash filtration is performed 1-2 times.

상기, 세척이 끝난 진주고형분에 5 ∼ 20%의 식용빙초산 수용액을 천천히첨가하면서 350 ∼ 600rpm으로 교반한다. 이때 반응온도는 상온을 유지한다. 이산화탄소가 발생하지 않는 때를 반응이 끝난 것으로 보고 상등액(제1액)을 회수한다. 제1액은 초산칼슘을 포함한 투명-회백색의 투명한 수용액이다. 제1액의 양은 첨가하는 진주의 산지와 산의 농도에 따라 결정된다.The solution is stirred at 350 to 600 rpm while slowly adding 5-20% of an edible glacial acetic acid aqueous solution to the washed pearl solid. At this time, the reaction temperature is maintained at room temperature. When the reaction does not occur when carbon dioxide is generated, the supernatant (first liquid) is recovered. The first liquid is a clear-grey-white clear aqueous solution containing calcium acetate. The amount of the first liquid is determined according to the acid and concentration of the pearl to be added.

이 때 빙초산의 주성분은 초산(CH3COOH)이고, 진주의 주성분은 탄산칼슘(CaCO3)이므로 수용액에서 이들의 반응은 다음과 같이 이루어진다.At this time, the main component of glacial acetic acid is acetic acid (CH 3 COOH), the main component of pearl is calcium carbonate (CaCO 3 ), so their reaction in the aqueous solution is as follows.

CaCO3+ 2CH3COOH Ca(CH3COO)2+ H2O + CO2CaCO 3 + 2CH 3 COOH Ca (CH 3 COO) 2 + H 2 O + CO 2

결국 진주분말과 빙초산을 반응시켜 제조하는 수용성 진주칼슘의 주성분은 다량의 초산칼슘과 가수분해된 미량의 단백질이라 할 수 있다.After all, the main component of the water-soluble pearl calcium prepared by reacting pearl powder and glacial acetic acid is a large amount of calcium acetate and hydrolyzed trace protein.

제 1 단계 반응이 완료되면 상등액을 원심 또는 여과분리하고, 침전물을 정제수나 증류수로 여러 차례 세척하여 최종세척액의 pH가 중성이 되도록 한다.After completion of the first stage reaction, the supernatant is centrifuged or filtered off, and the precipitate is washed several times with purified or distilled water so that the pH of the final washing solution is neutral.

제 1 단계의 세척한 고형분에 2 ∼ 10배량의 정제수를 가하고 상온에서 350 ∼ 600rpm으로 1시간 교반하여 수용성 잔류성분을 용출시킨 다음 여과분리한다(제2액).2 to 10 times the amount of purified water was added to the washed solid of the first step, and the mixture was stirred at 350 to 600 rpm for 1 hour at room temperature to elute the water-soluble residual component and then separated by filtration (second solution).

상술한 제1액과 제2액을 혼합한 다음 직접 또는 묽은 알카리로 중화시킨 혼합수용액은 칼슘농도 20,000ppm이상, 단백질농도 0.1 ∼ 1.0㎎/㎖ 범위의 수용성진주용액을 제조한다(제3액).The first aqueous solution and the second liquid were mixed and then neutralized with direct or dilute alkaline solution to prepare an aqueous pearl solution with calcium concentration of 20,000 ppm or more and protein concentration of 0.1-1.0 mg / ml (third solution). .

상기, 제3액은 모든 건조방식을 이용하여 분말을 제조할 수 있으나, 바람직하게는 100 이상의 온도에서 분무 건조하여 수용성 진주분말을 제조한다. 이 분말은 그대로 이용할 수도 있으나, 기능성을 향상시키기 위하여 버섯다당체추출물, 뮤코다당단백, 실크아미노산, 비타민 D 등을 혼합하여 기능성의 수용성 진주분말을 제조한다.The third liquid may be prepared by using all drying methods, but preferably spray dried at a temperature of 100 or more to prepare a water-soluble pearl powder. This powder may be used as it is, but in order to improve functionality, a water-soluble pearl powder is prepared by mixing a mushroom polysaccharide extract, mucopolysaccharide protein, silk amino acid, vitamin D and the like.

진주에 포함된 칼슘의 농도는 원자흡광분석방법(ASS)이나 무기이온측정법으로, 단백질의 농도는 세미킬달법을 이용하여 측정하였다.The concentration of calcium in pearls was measured by atomic absorption spectrometry (ASS) or inorganic ion measurement, and the concentration of protein was measured using semi-Kjeldahl method.

이하 제조예 및 실시예를 통하여 본 발명을 좀 더 구체적으로 설명하지만 아래 실시예에 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.

실시예 1. 물리적 방법(전처리 제조예 1)Example 1 Physical Method (Pretreatment Preparation Example 1)

양식 바다진주와 민물진주 각각 50g씩을 2개의 용기에 담고, 정제수 또는 증류수를 2 ∼ 3배량을 첨가한 후 잘 혼합한 다음 방치하여 상등액을 제거하고, 같은 방법으로 2 ∼ 3회를 반복하여 원심분리 또는 여과 세척하여 고형분을 분리한다.50g each of cultured sea pearls and freshwater pearls are placed in two containers, 2 ~ 3 times of purified water or distilled water is added, mixed well, then left to remove the supernatant, and centrifuged 2 ~ 3 times in the same manner. Or by filtration washing to separate the solids.

실시예 2. 화학적 방법(산가수분해 제조예 2)Example 2. Chemical Method (Acid Hydrolysis Preparation Example 2)

제조예 1에서 얻은 고형분 100g에 7% 식용빙초산 약 400㎖를 천천히 첨가한다.About 400 ml of 7% edible glacial acetic acid was slowly added to 100 g of the solid obtained in Preparation Example 1.

혼합과 교반장치를 이용하였고, 반응온도는 상온이였다. 기포가 더 이상 발생하지 않고 황색의 액체가 생성되면 이것을 상온까지 냉각하여 진주칼슘-초산염(액체)와 나머지 불용성 물질(고형분)으로 나누어진다. 약 2-3시간 정도 반응시켜 1300㎖의 투명한 수용액을 여과 분리하였다(제2액). 제2액은 20,000ppm의 칼슘과 소량의 단백질이 함유되어 있다. 제2액을 제조하면서 발생한 고형분에 약 2 ∼ 3배량의 정제수나 증류수로 2 ∼ 3회 세척하여 최종세척수의 pH가 중성이 될 때까지이 과정을 반복한다.Mixing and stirring were used, and the reaction temperature was room temperature. When bubbles no longer occur and a yellow liquid is produced, it is cooled to room temperature and divided into pearl calcium-acetate (liquid) and the remaining insoluble matter (solid content). After reacting for about 2-3 hours, 1300 ml of a clear aqueous solution was separated by filtration (second solution). The second solution contains 20,000 ppm of calcium and a small amount of protein. Repeat this process until the pH of the final wash water is neutralized by washing it 2-3 times with about 2-3 times the amount of purified water or distilled water.

실시예 3, 건조분말제조(수용성 진주칼슘 및 단백질함유 분말)Example 3, dry powder preparation (water soluble calcium and protein-containing powder)

제조 예2와 예3에서 얻은 용액을 분무 건조하여 수용성 진주칼슘 및 단백질 분말을 제조하였다. 상기 방법으로 제조한 수용성 진주칼슘분말은 원료대비 중량으로 0.8 ∼ 0.95이 얻어졌다.Water-soluble pearl calcium and protein powder were prepared by spray drying the solutions obtained in Preparation Examples 2 and 3. Water-soluble pearl calcium powder prepared by the above method was obtained 0.8 ~ 0.95 by weight relative to the raw material.

실시예 4. 수용성 진주칼슘과 기능성 성분을 함유한 분말제조Example 4 Preparation of Powder Containing Water Soluble Pearl Calcium and Functional Ingredient

상기, 실시예 1에서 얻은 분말과 버섯다당체 추출물, 뮤코다당단백, 실크아미노산, 비타민 D 등을 혼합하여 기능성의 수용성 진주분말을 제조하였다.To prepare a functional water-soluble pearl powder by mixing the powder obtained in Example 1, mushroom polysaccharide extract, mucopolysaccharide protein, silk amino acid, vitamin D and the like.

따라서, 본 발명은 물리적 및 화학적 방법을 이용하여 수용성 진주분말을 제조함으로써 칼슘과 활성단백질의 함량을 높일 수 있다.Therefore, the present invention can increase the content of calcium and active protein by preparing a water-soluble pearl powder using physical and chemical methods.

또한, 버섯다당체추출물, 뮤코다당단백, 실크아미노산, 비타민 D 등을 혼합하여 체내 칼슘흡수율을 높이고 면역강화와 피부노화를 방지할 수 있는 효과가 있다.In addition, mushroom polysaccharide extract, mucopolysaccharide protein, silk amino acid, vitamin D, etc. are mixed to increase the body's calcium absorption rate, it has the effect of preventing immune strengthening and skin aging.

Claims (5)

진주를 500 ∼ 1,000메쉬의 입자크기로 분쇄한 다음, 상온에서 2 ∼ 3배량의 물을 가해 여과 세척하여 얻은 고형분에 식용빙초산 수용액을 첨가하여 이산화탄소가 발생하지 않을 때까지 350 ∼ 600rpm으로 반응시킨 다음 고형분을 침전시키고 제1액을 분리하는 제 1 단계;The pearls were pulverized to a particle size of 500 to 1,000 mesh, and then edible glacial acetic acid aqueous solution was added to the solid obtained by filtration and washing at 2 to 3 times the water at room temperature, and then reacted at 350 to 600 rpm until no carbon dioxide was generated. A first step of precipitating solids and separating the first liquid; 상기, 제 1 단계에서 얻은 고형분에 정제수를 가해 반응시켜 잔류하는 수용성분을 분리하는 제 2 단계;A second step of separating purified water by adding purified water to the solid content obtained in the first step and reacting the reaction; 상기, 제1액과 제2액을 혼합하여 분무 건조하여 수용성 진주칼슘 및 단백질분말을 제조하는 제 3 단계;A third step of preparing a water-soluble pearl calcium and a protein powder by mixing the first liquid and the second liquid by spray drying; 상기, 제3단계에서 얻은 분말에 버섯다당체추출물, 뮤코다당단백, 실크아미노산, 비타민 D 등을 혼합하여 제조하는 것을 특징으로 하는 상온 산가수분해법을 이용한 수용성 진주분말의 제조방법.Method for producing a water-soluble pearl powder using the acid hydrolysis method at room temperature, characterized in that the powder obtained in the third step, the mushroom polysaccharide extract, mucopolysaccharide protein, silk amino acid, vitamin D and the like is prepared by mixing. 제 1 항에 있어서,The method of claim 1, 진주는 자연산 민물 양식이나, 바다양식 진주로 하고 상온에서 물리 및 화학적 방법을 이용하여 제조하는 것을 특징으로 하는 상온 산가수분해법을 이용한 수용선 진주분말의 제조방법.Pearl is a natural freshwater culture, or a sea-cultured pearl, the method of producing a water-line pearl powder using the acid hydrolysis method at room temperature, characterized in that it is produced using physical and chemical methods. 제 1 항에 있어서,The method of claim 1, 상기, 식용빙초산수용액의 농도가 1 ∼ 20%(v/v)임을 특징으로 하는 상온 산가수분해법을 이용한 수용성 진주분말의 제조방법.The method of producing a water-soluble pearl powder using an acid hydrolysis method at room temperature, characterized in that the concentration of the edible glacial acetic acid solution is 1 to 20% (v / v). 제 1 항에 있어서,The method of claim 1, 상기, 제 2 단계의 반응온도가 상온임을 특징으로 하는 상온 산가수분해법을 이용한 수용성 진주분말의 제조방법.The method for producing a water-soluble pearl powder using an acid hydrolysis method at room temperature, characterized in that the reaction temperature of the second step is room temperature. 제 1 항에 있어서,The method of claim 1, 상기, 식용빙초산 수용액이외에 농도가 1 ∼ 20%(v/v)인 젖산, 구연산, 코지산, 글리콜산 등의 유기산을 단독 또는 빙초산과 혼합하여 반응시킨 것을 특징으로 하는 상온 산가수분해법을 이용한 수용성 진주분말의 제조방법.In addition to the edible glacial acetic acid aqueous solution, water-soluble using the acidic hydrolysis method at room temperature, characterized by reacting an organic acid such as lactic acid, citric acid, kojic acid, glycolic acid having a concentration of 1 to 20% (v / v) alone or by mixing with glacial acetic acid. Method for preparing pearl powder.
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KR101223193B1 (en) * 2010-11-17 2013-01-17 김영섭 Water soluble pearl powder process
KR101706598B1 (en) * 2015-11-20 2017-02-15 인제대학교 산학협력단 Composition comprising water-soluble fructooligosaccharide calcium for preventing or treating bone disease and joint disease
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CN114886830B (en) * 2022-03-11 2024-06-04 广州澳谷化妆品制造有限公司 Scalp/hair/skin repairing composition using seawater pearl as raw material, preparation method and application thereof

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