KR960004497B1 - Liquid detergent composition containing enzyme - Google Patents
Liquid detergent composition containing enzyme Download PDFInfo
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- KR960004497B1 KR960004497B1 KR1019930017063A KR930017063A KR960004497B1 KR 960004497 B1 KR960004497 B1 KR 960004497B1 KR 1019930017063 A KR1019930017063 A KR 1019930017063A KR 930017063 A KR930017063 A KR 930017063A KR 960004497 B1 KR960004497 B1 KR 960004497B1
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38681—Chemically modified or immobilised enzymes
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2065—Polyhydric alcohols
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38627—Preparations containing enzymes, e.g. protease or amylase containing lipase
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2041—Dihydric alcohols
- C11D3/2044—Dihydric alcohols linear
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
Abstract
Description
본 발명은 피부 안정성 및 사용감이 우수하고 효소의 장기 안정성이 우수한 효소 첨가 세정제 조성물에 관한 것이다. 더욱 상세히 설명하면 맥반석 분말에 효소를 흡착, 고정화시킨 맥반석 고정화 효소의 무수황산나트륨, 탄산수소나트륨등의 무기염 및 다가 알콜올 함유하는 액체 세정제 조성물에 관한 것이다.The present invention relates to an enzyme-added cleaning composition having excellent skin stability and usability and excellent long-term stability of the enzyme. More specifically, the present invention relates to a liquid detergent composition containing inorganic salts such as anhydrous sodium sulfate, sodium hydrogen carbonate, and polyhydric alcoholol of an adsorbed and immobilized enzyme on elvan rock powder.
일반적으로, 지방질이나 무기물에 의한 오염은 비누, 세제등의 세정제에 의해 쉽게 제거되지만 신체나 피복중의 단백질에 의한 오염은 쉽게 제거되지 않는 단점이 있기 때문에 비누나 세제등에 효소를 첨가하여 세정 효과를 높이는 방법이 연구되어 왔다. 효소는 산성에서 안정하고 알칼리에서 쉽게 활성을 잃기 때문에 비누 및 액체 세정제에서의 사용이 제한 받아 왔지만 알칼리에서 안정한 효소를 이용한 여러 방법이 연구되고 실용화되고 있다.In general, contamination by fats or minerals is easily removed by detergents such as soaps and detergents, but contamination by proteins in the body and coating is not easily removed. Therefore, enzymes may be added to soaps or detergents to provide a cleaning effect. How to increase has been studied. Although enzymes are stable in acidity and easily lose their activity in alkalis, their use in soap and liquid detergents has been limited, but several methods using enzymes stable in alkalis have been studied and put into practice.
예를 들면, 노보(Novo)의 유럽특허 EP 0214761호 및 EP 0258068호에서는 미생물로부터 추출한 리파아제에 대한 상세한 설명 및 세제에 첨가한 예들이 기재되어 있고, 유니레버(Unilever)의 유럽특허 EP 0407225호에는 유전자 변이에 의해 알칼리에서 안정한 효소에 대한 제조법이 설명되어 있다. 그러나, 효소는 장기 보관시 효소가 잃기 쉽고 피부자극등의 부작용이 생길 수 있으며, 유전자 변이등도 실용화하기에 번거로운 단점들이 있다.For example, Novo's European Patents EP 0214761 and EP 0258068 describe detailed descriptions of lipases extracted from microorganisms and examples added to detergents, and Unilever's European Patent EP 0407225 describes genes. Variation describes the preparation for enzymes that are stable in alkali. However, enzymes are prone to loss of enzymes and prolonged side effects such as skin irritation during long-term storage, and gene mutations are also cumbersome for practical use.
또한, 효소는 분말이나 고형상태로 존재하는 것보다 수용액중에서 쉽게 활성을 잃는 경향이 있는데 이는 물분자가 효소의 펩티드 결합을 가수분해해서 활성을 잃게 하는 것으로 알려져 있고, 음이온 계면활성제등에 의해서도 안정성이 저하된다.In addition, enzymes tend to lose their activity in aqueous solutions more easily than they exist in powder or solid state, which is known to cause water molecules to lose activity by hydrolyzing the peptide bonds of enzymes. do.
수용액중에서 효소의 안정성을 높이기 위해서는 폴리에틸렌글리콜, 프로필렌글리콜, 글리세린, 솔비톨등의 다가 알콜을 첨가하여 효소의 펩티드 결합을 공격하는 물분자를 봉쇄하는 방법이 많이 사용되고 있으나 장기 보관시 안정성이 좋지 않는 단점이 있다.In order to increase the stability of enzymes in aqueous solution, polyhydric alcohols such as polyethylene glycol, propylene glycol, glycerin and sorbitol are added to block water molecules that attack peptide bonds of enzymes. have.
이에 본 발명자들은 맥반석이 일반적으로 다공성의 물질로 노폐물 흡수작용이 있어 세안이나 입욕시 사용하면 피부유연효과 및 노화방지등에 효과가 있다는 사실에 착안하여 연구를 계속 하던중, 효소를 물불용성인 맥반석 분말에 흡착고정시키고 다가 알콜 및 무기염을 혼합하였더니 효소의 안정성이 향상되고 피부자극이 현저히 감소된다는 사실을 밝혀내고 본 발명을 완성하게 되었다.Accordingly, the present inventors have focused on the fact that elvan is generally a porous substance, and has an absorbing effect of waste products, so that it is effective in skin softening effect and anti-aging when used in washing or bathing. After the adsorption fixation and the polyhydric alcohol and the inorganic salt were mixed, it was found that the stability of the enzyme was improved and the skin irritation was significantly reduced, thereby completing the present invention.
본 발명은 맥반석에 알칼리 프로테아제와 파파인 0.1 내지 10중량부를 흡착시킨 맥반석 고정화 효소 0.1 내지 10중량부, 다가 알콜 10 내지 20중량부 및 무기염 5 내지 15중량부를 함유함을 특징으로 하는 세정제 조성물을 제공한다.The present invention provides a detergent composition comprising 0.1 to 10 parts by weight of ganbanite immobilizing enzyme, 10 to 20 parts by weight of polyhydric alcohol, and 5 to 15 parts by weight of inorganic salts, adsorbing 0.1 to 10 parts by weight of alkaline protease and papain on gannet. do.
본 발명은 또한 맥반석에 알칼리 프로테아제, 파파인 및 라파아제 0.1 내지 10중량부를 흡착시킨 맥반석 고정화 효소 0.1 내지 10중량부, 다가 알콜 10 내지 20중량부 및 무기염 5 내지 15중량부를 함유함을 특징으로 하는 세정제 조성물을 제공한다.The present invention is also characterized in that it contains 0.1 to 10 parts by weight of elvan immobilized enzyme, 10 to 20 parts by weight of polyhydric alcohol, and 5 to 15 parts by weight of inorganic salts, which are adsorbed on 0.1 to 10 parts by weight of alkali protease, papain and rapase. It provides a detergent composition.
본 발명에 따른 세정제 조성물에 있어서, 다가 알콜은 프로필렌글리콜, 폴리에틸렌글리콜, 솔비톨 또는 글리세린이 바람직하게 사용되고, 무기염은 무수황산나트륨, 탄산나트륨 또는 탄산수소나트륨이 바람직하게 사용된다.In the cleaning composition according to the present invention, the polyhydric alcohol is preferably propylene glycol, polyethylene glycol, sorbitol or glycerin, and the inorganic salt is preferably anhydrous sodium sulfate, sodium carbonate or sodium hydrogencarbonate.
본 발명의 세정제 조성물중에 사용되는 효소는 단백질 분해효소인 프로테아제 및 파파인이 바람직하며, 계면활성제가 없는 세정제에는 지방질 분해효소인 리파아제를 50% 혼합 사용하는 것이 바람직하다. 프로테아제는 동물계 단백질 분해 효소로서 산성에서 활성이 최대이나 알칼리 프로테아제를 사용하면 중성이나 알칼리에서 높은 활성을 보여준다. 파파인은 식물계 단백질 분해 효소로서 산성, 중성 및 알칼리에서도 높은 활성을 가지고 있는 것으로 알려져 있다. 효소를 맥반석에 흡착시키는 방법은 순수한 물 500ml에 맥반석 25g과 단백질 및 지방질 분해효소 0.1 내지 10중량부를 첨가한 후 4℃에서 30분간 교반하여 효소가 맥반석에 충분히 흡착된 거름종이로 걸러 잔류물을 이용하는 방법을 사용할 수 있다.The enzyme used in the cleaning composition of the present invention is preferably a protease and papain, which are proteolytic enzymes, and 50% of a lipase, which is a lipolytic enzyme, is preferably used in the cleaning agent without a surfactant. Protease is an animal-based proteolytic enzyme, which shows the highest activity in acid but high activity in neutral and alkali when alkaline protease is used. Papain is a plant-based proteolytic enzyme that is known to have high activity in acid, neutral and alkali. The method of adsorbing enzyme to elvan is performed by adding 25 g of elvan and 0.1-10 parts by weight of protein and lipolytic enzyme to 500 ml of pure water, and then stirring it for 30 minutes at 4 ° C. to filter out the residue by filtering paper with enzyme sufficiently adsorbed on elvan. Method can be used.
본 발명에 따른 세정제 조성물은 피부보호 및 혈액순환을 촉진시켜 피로회복에 효과가 있는 감초, 당귀 및 은행 추출물중에서 선택된 1종 또는 2종 이상의 한방 성분을 추가로 함유시키는 경우 사용감이 크게 개선되는 것으로 나타났다.The cleaning composition according to the present invention has been found to greatly improve the feeling of use when it further contains one or two or more herbal ingredients selected from licorice, Angelica and ginkgo biloba extracts, which are effective for fatigue recovery by promoting skin protection and blood circulation. .
본 발명에 따른 세정제 조성물은 하이드록실기를 여러개 갖고 있는 비이온 계면활성제인 알킬폴리 글루코사이드(APG)를 첨가하는 경우 효소의 안정성 및 피부 자극에 큰 영향이 없고 세정력도 향상되는 것으로 나타났다. 세정력을 향상시키기 위해 사용되는 알킬폴리글루코사이드(APG)는 다음 일반식과 같이 탄소수 8부터 14까지 글루코오스 단위가 2.3 이하인 것이 바람직하다.In the detergent composition according to the present invention, when the alkyl poly glucoside (APG), which is a nonionic surfactant having several hydroxyl groups, was added, the detergent composition and the skin irritation were not significantly affected, and the cleaning power was also improved. The alkylpolyglucoside (APG) used to improve the detergency is preferably a glucose unit having 2.3 or less carbon atoms from 8 to 14, as shown in the following general formula.
더욱 구체적으로, 본 발명의 세정제 조성물은 이온수 40 내지 60중량부에 피부유연효과 및 혈액순환 촉진효과가 있는 감초, 당귀, 은행 추출물 5 내지 20중량부를 단독 또는 혼합사용하고 프로필렌글리콜, 폴리에틸렌글리콜, 솔비톨, 글리세린 등의 다가 알콜 10 내지 20중량부, 무수황산나트륨, 탄산나트륨, 탄산수소나트륨 등의 무기염 5 내지 15중량부, 맥반석 고정화 효소 0.1 내지 10중량부를 사용하는 세정제 및 알킬폴리글루코사이드(APG) 또는 지방산칼륨 1 내지 10중량부를 함유하는 세안 및 입욕 겸용 액체 세정제이다.More specifically, the cleaning composition of the present invention is used alone or mixed 5 to 20 parts by weight of licorice, Angelica, ginkgo extract having skin softening effect and blood circulation promoting effect to 40 to 60 parts by weight of ionized water, propylene glycol, polyethylene glycol, sorbitol , 10 to 20 parts by weight of polyhydric alcohols such as glycerin, 5 to 15 parts by weight of inorganic salts such as anhydrous sodium sulfate, sodium carbonate and sodium hydrogen carbonate, 0.1 to 10 parts by weight of ganbanite immobilizing enzyme and alkyl polyglucoside (APG) or fatty acid A face wash and bath liquid cleaning agent containing 1 to 10 parts by weight of potassium.
맥반석 고정화 효소를 0.1중량부 미만 사용시에는 세정효과를 느끼기 어렵고, 10중량부 이상 사용하면 사용감이 떨어지고 피부자극등의 단점이 생길 수 있다. 또한, 한방성분 및 무기염을 5중량부 미만 사용할 경우 피부유연효과가 줄어들고 한방성분은 20중량부 이상 사용시 사용감이 저하되고 무기염은 15중량부 이상 사용시 결정으로 석출되는 단점이 있다.When using less than 0.1 parts by weight of elvan immobilized enzyme is difficult to feel the cleaning effect, when used more than 10 parts by weight may cause a decrease in the feeling of use and skin irritation. In addition, when using less than 5 parts by weight of herbal components and inorganic salts, the skin softening effect is reduced, the herbal components have a disadvantage in that the feeling of use decreases when using more than 20 parts by weight and the inorganic salts are precipitated as crystals when used in more than 15 parts by weight.
이하 실시예에 의거하여 본 발명을 더욱 상세히 설명한다.The present invention will be described in more detail with reference to the following examples.
[실시예]EXAMPLE
다음 표 1과 같은 조성을 갖는 세제 조성물을 제조하였다.Next, a detergent composition having the composition shown in Table 1 was prepared.
상기 표 1에서 사용된 지방산 칼륨은 라우릴산 칼륨과 미리스틴산 칼륨을 사용했고 효소의 구성비는 다음 표 2와 같다.The fatty acid potassium used in Table 1 used potassium lauryl acid and potassium myristic acid, and the composition ratio of the enzyme is shown in Table 2 below.
상기 실시예 1 내지 3 및 비교예 1 내지 3의 세정제 조성물에 대한 피부안정성 및 장기 보관시 안정성은 다음과 같이 실험하였다.Skin stability and long-term storage stability of the cleaning composition of Examples 1 to 3 and Comparative Examples 1 to 3 were tested as follows.
(1) 피부 안정성 실험(1) skin stability test
실시예 및 비교예의 세정제들의 피부 안정성을 측정하기 위해 성인 남녀 20명의 팔에 24시간 동안 8% 용액으로 패키 테스트(Patch test)를 실시한 후, 육안으로 자극도를 판정한 결과는 다음 표 3과 같다.In order to measure the skin stability of the cleaning agents of the Examples and Comparative Examples after performing a patch test with 8% solution for 24 hours on the arms of 20 adult men and women, the result of visually determining the degree of stimulation is shown in Table 3 below. .
수치는 인원수를 나타내며 등급은 다음과 같다.The figures represent the number of people and the classes are as follows:
- : 정상 ± : 경미한 홍반-: Normal ±: Mild erythema
+ : 홍반 ++ : 홍반 및 부종+: Erythema ++: erythema and edema
상기 표 3으로부터, 실제 느끼는 자극은 +이상으로 효소를 맥반석에 흡착 고정화 시킴으로서 자극이 현저히 감소하는 것은 알 수 있고, 음이온 계면활성제(칼륨비누)에 비해 알킬폴리글루코사이드가 자극이 경미하다는 것을 알 수 있다.From the above Table 3, it can be seen that the stimulation is actually reduced by the adsorption and immobilization of the enzyme to the ganban rock more than +, the stimulation of the alkyl polyglucoside is mild compared to the anionic surfactant (potassium soap). .
(2) 장기 보관시 안정성 실험(2) Long-term storage stability test
장기 보관시 안정성을 실험하기 위하여 50℃ 항온기에서 2주간 보관한 후 효소의 잔류 활성을 측정하기 위하여 단백질 분해능을 다음과 같이 실험했다. 먼저, 50℃ 항온조에서 시험관에 1% 소디움 설파이트(Na2SO3) 용액 50ml를 채우고 여기에 세정제 1ml를 가한 후 약 2분간 교반하였다. 0.4% N.N 디메틸 카제인(DMC) 2ml를 가한 후 교반하면 효소에 의해 디메틸카제인의 저분자 펩티드 결합이 분해되어 자유 아미노기가 유리된다. 여기에 0.1% 2,4,6-트리니트로벤젠설포닉에시드(TNBS) 0.5ml를 가하면 자유 아미노기와 반응하여 붉은색을 띄다가 점차 노란색으로 변한다. 이 시험관을 25℃로 냉각한 후 425nm에서 흡광도를 측정 비교하여 효소의 활성을 측정한 결과는 다음 표 4와 같다.In order to test the stability during long-term storage, the protein resolution was tested as follows to determine the residual activity of the enzyme after storing for 2 weeks in a 50 ℃ thermostat. First, 50 ml of a 1% sodium sulfite (Na 2 SO 3 ) solution was filled in a test tube in a 50 ° C. thermostat, and 1 ml of a detergent was added thereto, followed by stirring for about 2 minutes. After adding 2 ml of 0.4% NN dimethyl casein (DMC) and stirring, the low-molecular peptide bond of dimethyl casein is decomposed by the enzyme to free the free amino group. When 0.5 ml of 0.1% 2,4,6-trinitrobenzenesulfonic acid (TNBS) is added thereto, it reacts with free amino groups to become red and gradually turn yellow. The test tube was cooled to 25 ° C., and then the absorbance at 425 nm was measured to compare enzyme activity.
표준품 1은 실시예 1을, 표준품 2는 비교예 1을 실험전에 제조한 기준품이다. 수치는 표준품의 흡광도를 100으로 기준하여, 환산한 값이며, 효소를 맥반석에 흡착 고정화시킴으로서 안정성이 증가하고 음이온보다 알킬폴리글루코사이드를 사용했을때 안정성이 우수하다는 것을 알 수 있다.Standard 1 is Example 1, and Standard 2 is Comparative Example 1 prepared before the experiment. The numerical value is calculated based on the absorbance of the standard product based on 100, and it can be seen that the stability is increased by adsorbing and immobilizing the enzyme on the elvan, and the stability is better when the alkyl polyglucoside is used than the anion.
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