KR100804993B1 - Manufacturing method of toilet soap contained the extracts from seeds of paeonia lactiflora p - Google Patents

Manufacturing method of toilet soap contained the extracts from seeds of paeonia lactiflora p Download PDF

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KR100804993B1
KR100804993B1 KR1020070008701A KR20070008701A KR100804993B1 KR 100804993 B1 KR100804993 B1 KR 100804993B1 KR 1020070008701 A KR1020070008701 A KR 1020070008701A KR 20070008701 A KR20070008701 A KR 20070008701A KR 100804993 B1 KR100804993 B1 KR 100804993B1
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extract
gnetin
soap
paeonia lactiflora
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박준홍
배수곤
박현로
박석희
김규성
최장수
신정화
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경상북도 농업기술원
신정화
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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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/22—Organic compounds, e.g. vitamins
    • C11D9/38—Products in which the composition is not well defined
    • 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
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/10—Washing or bathing preparations
    • 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
    • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
    • C11D13/10—Mixing; Kneading
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74—Biological properties of particular ingredients

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Abstract

A method for preparing a beauty soap is provided to improve the skin whitening effect and the moisturizing effect by using Paeonia lactiflora Pall. and 1,3-butylene glycol. A method for preparing a beauty soap comprises the step of mixing 85-89 wt% of a soap base containing 12-25 wt% of moisture; 1 wt% of distilled water; 1 wt% of perfume; 8-12 wt% of 1,3-butylene glycol; and 1 wt% of an extract of the seed of Paeonia lactiflora Pall. which contains gnetin H. Preferably the extract of the seed of Paeonia lactiflora Pall. is prepared by removing an oil component from the seed of Paeonia lactiflora Pall. by using n-hexane; and extracting the obtained one by using 80% ethanol.

Description

작약종자 추출물을 이용한 화장비누 제조법 {Manufacturing method of toilet soap contained the extracts from seeds of Paeonia lactiflora P.}Manufacturing method of toilet soap using peony seed extract {Manufacturing method of toilet soap contained the extracts from seeds of Paeonia lactiflora P.}

도 1은 작약종자 추출물 이용한 화장비누 제조 공정을 도식화한 것이다Figure 1 is a schematic of the manufacturing process soap using peony seed extract.

도 2는 작약종자로부터 미백효능물질을 함유하고 있는 추출물 제조공정을 도식화한 것이다Figure 2 is a schematic of the extract manufacturing process containing the whitening effect material from peony seed

약용작물인 작약(Paeonia latiflora P.)은 주로 건조한 뿌리를 한약재로 많이 사용하고 있고, 주요 주요성분은 페오니플로린(paeoniflorin), 알비플로린(albiflorin), 페오놀(paeonol), 벤조산(benzoic acid) 등이며, 그 약리작용은 진경, 진통, 진정, 항경련, 항균작용 등으로 생약 감기약, 기능성식품 등의 생약재로도 많이 사용하고 있다. 그러나 최근 작약의 꽃에 달린 성숙 종자로부터 트란스-레즈베라트롤(trans-resvaratrol), 트란스-비니페린(trans-viniferin), 시스-비니페린(cis-viniferin), 서프루티코졸에이(suffruticosol A), 서프루티코졸비(suffruticosol B), 그네틴에이치(gnetin H)등의 생리활성물질이 발견되었으며, 이러한 성분들은 항암 및 항돌연변이 효과가 강한 것으로 알려져 있다. 특히 그네틴 에이치(Gnetin H)는 피부 멜라닌색소 생성에 관여하는 티로시네이즈(tyrosinase) 효소의 활성 억제능력이 매우 큰 것으로 알려져 있다.Medicinal crop Peony ( Paeonia latiflora P.) mainly uses dry root as a herbal medicine, and its main ingredients are paeoniflorin, albiflorin, paeonol, and benzoic acid. Its pharmacological action is used as a herbal medicine such as herbal medicine, cold medicine, functional food, etc. as a result of Jingyeong, analgesic, soothing, anticonvulsion, and antibacterial action. But recently, from the mature seeds on the flowers of the peony, trans-resvaratrol, trans-viniferin, cis-viniferin, suffruticosol A, Biologically active substances such as suffruticosol B and gnetin H have been found, and these components are known to have strong anticancer and antimutagenic effects. Particularly, it is known that GNETIN H has a very high activity inhibiting activity of tyrosinase enzyme, which is involved in skin melanin pigment production.

일반적으로 비누는 유지를 비누화반응시켜 수용성 알칼리 금속염을 주제로 하여 제조하는 것으로 그 형태에 따라 고체비누, 액체비누가 있으며, 그 용도에 따라 세안용 화장비누, 세탁, 세척을 주로 하는 공업용 비누로 구분된다. 국민소득 증대에 따른 생활수준의 향상으로 화장비누의 소비 취향은 비누의 단순한 피부의 청결보다는 피부에 영양을 공급함과 동시에 피부 미백, 여드름 치료 등 기능성이 가미된 화장비누를 선호하고 있다. 이와 같은 소비자의 욕구를 만족시키기 위하여 알로에, 감, 송이 추출물, 어성초, 천문동, 감초, 애기똥풀 등의 한약재 추출물, 미나리 추출물, 황토, 게르마늄 등을 첨가한 화장비누의 제조방법 등이 공지된 바 있다.In general, soaps are manufactured on the basis of water-soluble alkali metal salts by saponification of fats and oils, and there are solid soaps and liquid soaps according to their forms. do. Increasing the standard of living in line with the increase of national income, the consumption taste of cosmetic soap prefers cosmetic soaps with functionalities such as skin whitening and acne treatment, as well as nourishing the skin rather than clean skin of soap. In order to satisfy the consumer's desire, there has been known a method of preparing a cosmetic soap containing aloe, persimmon, matsutake extract, eosungcho, medicinal herb extract such as astronomical tract, licorice, celandine grass, buttercup extract, ocher, germanium and the like.

본 발명은 작약 종자로부터 그네틴에이치(gnetin H)를 함유하고 있는 추출물 제조방법과 이 추출물의 그네틴에이치(gnetin H)의 함량과 티로시네이즈(tyrosinase) 효능억제정도 확인 그리고 이 추출물을 이용한 화장비누를 제조함으로서, 한약재로 주로 사용되고 있는 작약의 활용도를 한층 더 진작시켜 작약 재배농가의 소득 증대와 건강하고 하얀 피부를 가지고 싶어 하는 소비자의 욕구를 충족시킬수 있는 세안용 화장비누를 개발하는데 발명의 목적이 있다.The present invention provides a method for producing an extract containing gnetin H from peony seeds, the content of gnetin H and the degree of inhibition of tyrosinase efficacy of the extract, and cosmetics using the extract. By manufacturing soap, the purpose of the invention is to further enhance the utilization of peony, which is mainly used as a herbal medicine, to develop face wash soaps that can meet the needs of consumers who want to increase income of peony farmers and have healthy white skin. have.

본 발명은 작약 종자로부터 미백효능물질로 알려진 그네틴에이치(gnetin H)를 함유하고 있는 추출물 제조방법과 피부 자극을 일으키는 트리에탄올아민(TEA)을 제거한 비누소지를 중탕한 용액에 부틸렌 글리콜(1,3-butylene glycol) 등의 혼합원료를 첨가한 후 다시 중탕하고 미백효능물질을 함유하고 있는 작약종자 추출물과 향을 일정비율로 첨가/혼합 제조하여 만든 완제품 화장비누가 세정시 피부 미백효과 및 보습에 의해 피부의 보호 및 개선효과를 가지는 기술적 과제를 두고 발명된 것이다.The present invention provides a method for preparing an extract containing gnetin H, which is known as a whitening active substance, from a peony seed, and a butylene glycol (1, 1) in a solution containing soaps free of triethanolamine (TEA), which causes skin irritation. After adding mixed raw materials such as 3-butylene glycol) and soaking them again, Peony seed extract containing whitening efficacy substance and the finished product cosmetic soap made by adding / mixing fragrance at a certain ratio are used for skin whitening effect and moisturizing. By the technical problem having the protection and improvement of the skin by the invention.

이하 본 발명의 작약종자로부터 미백효능물질을 함유하고 있는 추출물 제조공정과 이 추출물을 이용한 화장비누의 제조공정을 상세히 설명하면 아래와 같다.Hereinafter will be described in detail the manufacturing process of the extract containing the whitening active material from the peony seed of the present invention and the manufacturing process of the cosmetic soap using the extract as follows.

본 발명은 작약 종자로부터 그네틴에이치(gnetin H)를 함유하고 있는 추출물 제조방법(도2)과 이 추출물의 그네틴에이치(gnetin H) 함량과 티로시네이즈(tyrosinase) 효소활성 억제정도 확인 그리고 이 추출물을 이용한 화장비누를 제조방법(도1)에 대한 실시 예를 상세히 설명한다.The present invention provides a method for producing an extract containing gnetin H from peony seeds (Fig. 2), the gnetin H content and tyrosinase enzyme activity inhibition of the extract, and An embodiment of a method of manufacturing cosmetic soap using the extract (FIG. 1) will be described in detail.

실시예 1 : 작약종자로부터 그네틴에이치(gnetin H)를 함유하는 추출물 제조방법Example 1 Preparation Method of Extract containing Gnetin H from Peony Seed

작약 종자로부터 그네틴에이치(gnetin H)를 함유하고 있는 추출물 제조방법으로 더욱 상세하게는 약용작물인 작약 성숙종자를 채취하여 분쇄한 가루를 100％ 노르말 헥산에 넣어 3시간 동안 상온에 방치하여 상등액을 제거 한 후 잔여물만 남기고, 다시 이 잔여물을 100％ 노르말 헥산에 넣어 이러한 조작을 2회 더하여 작약 종자의 기름성분을 완전히 제거한다. 기름성분이 제거된 작약 종자의 잔여물을 80％ 에탄올 용액에 넣어 상온에서 2시간 동안 초음파 추출기(sonicator, Branson co.)로 추출한 후 여과지(whatman No.3)로 여과하여 얻은 추출액과 여과지에 남은 잔여물을 다시 80％ 에탄올 용액에 넣어 초음파 추출기로 추출하는 과정을 2회 더하여 얻은 추출액을 모아 감압농축기에 넣어 40℃에서 감압 농축하여 작약 종자의 추출물을 얻는다.A method for producing an extract containing gnetin H from peony seed, more specifically, extracting mature seed, a medicinal crop, and grinding the powder into 100% normal hexane and standing at room temperature for 3 hours for supernatant. After removal, only the residue is left, and the residue is added to 100% normal hexane again to add two such operations to completely remove the oil content of the peony seed. The residue of the oil-derived peony seed was extracted in an 80% ethanol solution and extracted with an ultrasonic extractor (sonicator, Branson co.) For 2 hours at room temperature, and then filtered through a filter paper (whatman No. 3). The residue was added again to the 80% ethanol solution and the extract was extracted twice with an ultrasonic extractor. The extract was collected and put into a vacuum condenser and concentrated under reduced pressure at 40 ° C to obtain an extract of peony seed.

실시예 2 : 작약종자 추출물의 그네틴에이치(gnetin H) 함량과 티로시네이즈 저해활성 효과Example 2 Gnetin H Content and Tyrosinase Inhibitory Effect of Peony Seed Extract

작약종자에서 미백효능이 우수한 그네틴에이치(gnetin H) 함량이 높은 채취시기를 구명하기 위하여 경상북도농업기술원 신물질연구소에서 8월 중순부터 9월 하순까지 작약종자를 시기별로 채취하여 음건한 후 에탄올로 추출한 추출물의 그네틴에이치(gnetin H)의 함량을 분석하였으며, 분석방법은 다음과 같다.In order to investigate the harvesting time of high whitening effect of high gnetin H in Peony seeds, Peony seeds were harvested from mid-August to late September by Gyeongsangbuk-do Agricultural Research and Extension Services, and dried with ethanol. Gnetin H content of the extract was analyzed, and the analysis method was as follows.

작약종자 분쇄시료 1g을 100％ 노르말 헥산으로 탈지한 후 80％ 에탄올 30㎖를 첨가하고 2시간 동안 초음파추출기로 추출하여 0.45㎛ 멤브레인 필터(membrane filter)로 여과한후 액체크로마토그래프(high performance liquid chromatograph)로 분석하였다. 분석용 칼럼은 오디에스에이칼럼(ODS-A column, 4.6×250mm, 5㎛), 검출기는 피디에이검출기(PDA detector)로 320nm에서 측정하였으며 이동상은 20％ 메탄올과 100％ 메탄올을 이용하여 용매기울기법으로 분석하였다.1 g of Peony seed crushed sample was degreased with 100% normal hexane, 30 mL of 80% ethanol was added, extracted with an ultrasonic extractor for 2 hours, filtered through a 0.45 μm membrane filter, and then subjected to a high performance liquid chromatograph. ). The analytical column was measured at 320 nm using an ODS-A column (4.6 × 250 mm, 5 μm), and the detector was a PDA detector. The mobile phase was a solvent gradient method using 20% methanol and 100% methanol. Analyzed.

[표 1] 작약종자에서 분리한 미백효능물질인 그네틴에이치(gnetin H)의 채취시기별 함량[Table 1] Content of harvesting time of gnetin H, a whitening agent isolated from peony seeds

Figure 112007500898797-pat00001
Figure 112007500898797-pat00001

작약종자 채취시기별 그네틴에이치(gnetin H) 함량 분석 결과 9월 15일, 9월 30일에서 각각 2.08％, 2.03％를 나타내어 9월 중하순에 작약 종자를 채취하는 것이 미백활성물질인 그네틴에이치(gnetin H)의 이용 측면에서 적절할 것으로 판단되었다.As a result of analysis of gnetin H content according to the time of harvesting peony seeds, 2.08% and 2.03% were shown on September 15 and September 30, respectively. (gnetin H) was considered appropriate in terms of use.

상기 작약종자에서 분리한 그네틴에이치(gnetin H)의 티로시네이즈 저해활성은 다음과 같은 방법으로 조사하였다. 50mM 소듐포스페이트 버퍼(sodium phosphate buffer, pH6.8) 620㎕에 5mM 도파(L-DOPA)를 녹인 기질액 200㎕ 및 시료용액 100㎕의 혼합액에 머쉬룸 티로시네이즈(mushroom tyrosinase, 120units/ml) 80㎕를 첨가하여 37℃에서 2분간 반응시켜 반응액 중에 생성된 도파크롬(DOPA chrome)을 475nm에서의 흡광도를 측정하였다. 티로시네이즈(tyrosinase) 저해활성은 시료용액의 첨가구와 무첨가구의 흡광도 감소율로 나타내었으며 아래의 수학식에 의하여 계산하였다.Tyrosinase inhibitory activity of gnetin H isolated from the peony seed was investigated in the following manner. Mushroom tyrosinase (120 units / ml) 80 ml of a substrate solution of 200 μl of 5 mM dopa (L-DOPA) dissolved in 620 μl of 50 mM sodium phosphate buffer (pH 6.8) and 100 μl of sample solution. The reaction mixture was added for 2 μl at 37 ° C., and the absorbance at 475 nm was measured for dopa chrome produced in the reaction solution. The tyrosinase inhibitory activity was expressed as a decrease in absorbance of the added and non-added samples of the sample solution and was calculated by the following equation.

[수학식][Equation]

Figure 112007500898797-pat00002
Figure 112007500898797-pat00002

[표 2] 그네틴에이치(Gnetin H)의 농도별 티로시네이즈 저해활성 효과[Table 2] Tyrosinase Inhibitory Effect of Gynetin H (Gnetin H) by Concentration

Figure 112007500898797-pat00003
Figure 112007500898797-pat00003

작약종자에서 분리한 그네틴에이치(gnetin H)의 농도별 티로시네이즈 저해활성 효과는 표 2와 같이 100ppm에서 76.1％의 억제율을 나타내어 기존의 미백활성 물질인 코직산 45％보다 우수한 활성을 나타내었다. 본 발명에 사용된 작약종자는 9월 하순에 채취한 종자로써 에탄올 추출물 1중량％로 첨가하여 만든 비누 1개에는 결과적으로 200ppm의 그네틴에이치(gnetin H)이 첨가되어 있다.Tyrosinase inhibitory effect of each concentration of gnetin H isolated from the peony seed showed an inhibition rate of 76.1% at 100 ppm as shown in Table 2, which was superior to 45% of kojic acid, a conventional whitening active substance. The peony seed used in the present invention was a seed collected in late September, and a soap made by adding 1% by weight of ethanol extract was added with 200 ppm of gnetin H as a result.

실시예 3 : 작약종자 추출물을 이용한 화장비누의 제조방법Example 3 Preparation of Cosmetic Soap Using Peony Seed Extract

작약종자 추출물을 이용한 화장비누 제조방법으로 더욱 상세하게는 실시 1과 같이 얻은 작약 종자의 에탄올 추출물의 시료를 물에 1:1 비율로 용해 희석시켜 미리 제조해 두고, 피부 자극을 일으키는 트리에탄올아민(TEA)을 제거한 비누소지를 60℃에서 3∼5시간 중탕한 후 화장비누 제조에 부틸렌 글리콜(1,3-butylene glycol) 등의 혼합원료를 첨가하여 2시간 더 중탕시킨다. 이 중탕된 비누용액에 상기 작약종자의 에탄올 추출물 희석액과 향료를 넣어 30분 동안 더 중탕한다. 완성된 비누용액을 성형 틀에 옮겨 담아 일주일 정도 자연 건조시킨 후 일정한 크기로 절단하고 금형 작업하여 완제품을 완성시킨다. 즉 일정한 방식으로 추출한 작약종 자의 에탄올 추출물을 주원료로 한 화장비누의 제조방법으로 상기 완성된 비누는 수분함량 12∼25중량％를 함유한 비누소지 85∼89중량％에 작약종자의 추출물 1중량％, 증류수 1중량％, 향 1중량％ 및 보습력이 뛰어난 부틸렌 글리콜(1,3-butylene glycol) 8∼12％중량의 비율로 혼합하여 제조한다.In more detail, the method of manufacturing cosmetic soap using peony seed extract was prepared by dissolving and diluting a sample of the ethanol extract of peony seed obtained in Example 1 in water at a ratio of 1: 1 and inducing triethanolamine (TEA). After removing the soap), the soap was bathed at 60 ° C. for 3 to 5 hours, and then a mixed raw material such as butylene glycol (1,3-butylene glycol) was added to make soap for 2 hours. Put the diluted ethanol extract and fragrance of the peony seed in this bath soap solution for 30 minutes more bath. Transfer the finished soap solution to the mold and let it dry for about a week, then cut it to a certain size and work on the mold to complete the finished product. In other words, the method of producing a cosmetic soap using the ethanol extract of peony seed extracted in a certain manner as the main ingredient is 85 to 89% by weight of soap content containing 12 to 25% by weight of water extract of Peony seed 1% by weight 1% by weight of distilled water, 1% by weight of fragrance and excellent moisturizing properties of 1,3-butylene glycol are prepared by mixing at a ratio of 8 to 12% by weight.

이와 같이 본 발명은 작약종자로부터 얻은 미백효능물질인 그네틴에이치(gnetin H)를 함유하고 있는 추출물을 첨가한 화장비누는 세안 시 피부미백효과와 동시에 통상적인 화장비누와는 달리 상기 비누 제조공정상 부틸렌 글리콜(1,3-butylene glycol)에 의한 보습효과가 뛰어나므로 본 발명의 화장비누를 제공함으로서 피부의 보호 및 개선 효과를 얻을 수 있음에 그 장점이 있다.As described above, the present invention provides a cosmetic soap containing an extract containing a whitening activator, gnetin H, which is obtained from a peony seed. Because of excellent moisturizing effect by lene glycol (1,3-butylene glycol) has the advantage that by providing a cosmetic soap of the present invention can obtain a protective and improving effect of the skin.

Claims (3)

삭제delete 수분함량 12∼25중량％를 함유한 비누소지 85∼89중량％에 증류수 1중량％, 향 1중량％, 보습력이 뛰어난 부틸렌 글리콜(1,3-butylene glycol) 8∼12중량％ 및 미백효능을 가지는 그네틴에이치(gnetin H)가 함유된 작약종자 추출물 1중량％를 포함하는 것을 특징으로 하는 화장비누의 제조법85 to 89% by weight of soap containing 12 to 25% by weight of water, 1% by weight of distilled water, 1% by weight, 8 to 12% by weight of moisturizing butylene glycol (1,3-butylene glycol) and whitening effect Method for producing a cosmetic soap, characterized in that it comprises a 1% by weight of the extract of Peony seed containing a ginein H (gnetin H) having a 청구항 2에 있어서, 작약 종자를 노르말 헥산으로 기름성분을 제거하고 80％ 에탄올로 추출하여 얻어진 미백효능물질 그네틴에이치(gnetin H)를 포함하는 작약 종자 추출물의 제조법The method according to claim 2, wherein the peony seed extract comprising gnetin H (whitening agent) obtained by removing the oil component with normal hexane and extracting with 80% ethanol is used.
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KR20130049040A (en) 2011-11-03 2013-05-13 (주)아모레퍼시픽 Cosmetic composition including taxifolin glucosides and extracting method of paeonia lactiflora extracts
KR101390465B1 (en) 2011-12-22 2014-05-07 (주)모아캠 Method for Preparing Paeonia lactiflora Extracts Containing Taxifolin-3-glucoside and Cosmetic Composition Containing Preparing Paeonia lactiflora Extracts
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