KR880000348B1 - Preparation of composition for rice-plant fever - Google Patents

Preparation of composition for rice-plant fever Download PDF

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KR880000348B1
KR880000348B1 KR1019850000709A KR850000709A KR880000348B1 KR 880000348 B1 KR880000348 B1 KR 880000348B1 KR 1019850000709 A KR1019850000709 A KR 1019850000709A KR 850000709 A KR850000709 A KR 850000709A KR 880000348 B1 KR880000348 B1 KR 880000348B1
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extracted
concd
acid
storage tank
hexane
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KR1019850000709A
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KR860006208A (en
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박병하
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박병하
이준섭
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]

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Abstract

An antifungal substance contg. caproic, bytric, n-valeric and iso- valeric acids was extd. from palslane (Portulacae Herba) and used for treating rice blast desease. Thus, palslane was steamboiled for 20- 30min at 100≰C > and pressed with a compressor to give palslance concentrate. The concentrate was extd. with MeOH and vacuum-concd.. The concd. ext. was dissolved in water. Water-sol. fraction was adjusted with HCl to pH 3.0 and extd. with ethylacetate and vacuum- concd.. The concd. ext. was extd. with nhexane, vacuum-concd., applied to Wacogel C-200 column, and eluted with n-hexane/ ethylacetate solvent system. The elute was pooled, concd., extd. with acetone, and concd. to give a white, oily material.

Description

카프로산, 부티르산, n-발레르산 및 이소발레르산으로 된 도열병 치료제의 제조 방법Method for preparing a cure for febrile disease consisting of caproic acid, butyric acid, n-valeric acid and isovaleric acid

본 발명은 카프로산, 부티르산, n-발레르산 및 이소발레르산으로 된 벼의 도열병 치료제의 제조 방법에 관한 것이다.The present invention relates to a method for the preparation of a therapeutic agent for rice blasts of rice consisting of caproic acid, butyric acid, n-valeric acid and isovaleric acid.

벼의 도열병을 방지 또는 치료하기 위하여 그동안 각종 농약을 사용하여 왔으나, 이러한 농약들은 화학적 제제였기 때문에 농부의 입, 피부 또는 흡인으로 인한 중독내지 약해가 대단하였으며, 그 사용법을 정확히 모르는 농민들의 잘못 사용으로 인하여 해마다 농약의 단위만 높아졌을 뿐만아니라, 천적이 멸종되어 생태계에서 큰 변화를 주었으며 또한 식물 자체에도 약해도 인한 결실의 감소 등 그 폐해가 대단히 컸었다.Various pesticides have been used to prevent or treat rice blasts, but since these pesticides were chemical preparations, they were very toxic or weakened by farmers' mouths, skin or aspirations. As a result, not only did the units of pesticides increase year by year, but also natural disasters caused extinction and caused great changes in the ecosystem.

또한 도열병을 예방 또는 치료하기 위하여 약제를 살포하여도 재발율이 높거나 유합율이 낮은 결점이 있었으며, 농약을 제조하기 위한 화학공장에서 나오는 폐기물 또는 개스로 공해가 더욱 격증된 페단등이 있었다.In addition, there was a drawback of high recurrence rate or low coalescence rate even when spraying drugs to prevent or treat febrile diseases, and pedan, which was further increased by waste or gas from chemical plants for producing pesticides.

본 발명은 이러한 종래의 페단을 일시에 시정함과 동시에 우리나라 산천에서 많이 생육되고 있는 야생초를 원료로 하여 인축에 전혀 약해가 없고 제발율이 없으며 공해를 동반하지 않는 이상적인 생약제의 도열병 치료제를 제조하는 방법에 관한 것이다.The present invention is to correct the conventional pedan at the same time and at the same time as a raw material of wild grasses that are grown a lot in the mountain of our country as raw materials, there is no harm to the killing rate, there is no rate and no method of manufacturing an antibacterial cure of an ideal herbal medicine It is about.

더우기 본 발명에 의한 치료제는 특히 벼의 도열병 치료에 탁월한 효과를 나타내며, 이밖에도 깨시 무늬병, 귀다리병, 갈색잎 마름병, 사과나무의 부란병 및 배나무의 검은 무늬병등에 탁월한 효과를 나타낸다.Moreover, the therapeutic agent according to the present invention exhibits an excellent effect, in particular, in the treatment of rice blast, and in addition, it has an excellent effect on sesame plaque, ear bud disease, brown leaf blight, apple blight and pear tree black.

특히 본 발명에 의한 치료제는 인축에 약해가 없으면서도 치료율이 높고 벼등 식물에도 약해를 주지 않을 뿐만 아니라 주제인 마치현이 우리나라의 산야에 많이 야생되고 있는 식물이라는 점에서 산업성이 우수한 치료제이다.In particular, the therapeutic agent according to the present invention is a therapeutic agent having excellent industrial properties in that it has a high cure rate and no harm to plants such as rice, but also has a weakness in human beings.

본 발명에 따른 도열병 치료제를 제조하기 위한 방법을 상세히 설명하면 다음과 같다.Referring to the method for producing a therapeutic agent for febrile disease according to the present invention in detail.

[제1공정][Step 1]

우리나라의 산이나 들에 많이 야생하는 마치현(馬齒

Figure kpo00001
: Portulacae Herba 일명 쇠비름)을 발육이 제일 양호한 7-8월경에 채취하여 뿌리를 제거하고 잘게 절단, 분쇄하여 저장탱크에 넣어 35℃-55℃의 온도로 24시간 마다 상하좌우로 잘 교반하면서 약 20일간 자연발효시킨 후, 찌꺼기가 나오지 않을 정도의 망을 사용하여 압축기로 압착하여 농축액을 추출한다.Machi prefecture wildly in Korea's mountains and fields
Figure kpo00001
: Portulacae Herba (aka Purslane) is harvested around July-August, which is best for development, and the roots are removed, finely chopped and pulverized and placed in a storage tank at a temperature of 35 ℃ -55 ℃ for 24 hours. After natural fermentation for a day, the extract is compressed by compressing with a compressor using a net that does not come out of the residue.

이와같은 공정대신에 마치현을 큰 가마솥에 넣어 100℃ 이상의 수증기로 20-30분간 찌거나, 마치현의 양에 비하여 약1/4정도의 물을 부어 100℃에서 20-30분간 삶은 후, 압축기로 압착하여 농축액을 추출하여 저장탱크에서 35℃-55℃의 온도로 20일간 자연발효를 시킬수도 있다.Instead of such a process, put the gusset into a large cauldron and steam it for 20-30 minutes with steam of 100 ℃ or more, or pour about 1/4 of water and boil it for 20-30 minutes at 100 ℃, then press it with a compressor. The extract can be extracted and fermented for 20 days at 35 ℃ -55 ℃ in a storage tank.

[제2공정][Step 2]

상기와 같은 공정으로 얻은 농축액에 메탄올을 첨가하여 용해된 성분을 추출하여 감압 농축하고 그 농축액에 물을 첨가하여 용해된 부분을 취해 염산으로 pH 3.0이 되도록 조절한 후 에틸 아세테이트로 추출하고 이 추출물을 감압 농축하여 농축액을 얻는다.Methanol was added to the concentrated solution obtained by the above-mentioned process to extract the dissolved component, concentrated under reduced pressure, the water was added to the concentrated solution, the dissolved portion was taken to adjust pH to 3.0 with hydrochloric acid, and extracted with ethyl acetate. Concentration under reduced pressure gives a concentrate.

[제3공정][Step 3]

이 농축액 중 n-헥산을 첨가하여 용해된 성분을 추출하여 감압 농축하고 이에 대해 규산 칼럼크로마토그래피를 실시한다.N-hexane is added to the concentrate to extract the dissolved components, and the residue is concentrated under reduced pressure, followed by silicate column chromatography.

이때 칼럼 충진제는“Wacogel C-200”이다.At this time, the column filler is "Wacogel C-200".

[제4공정][Step 4]

추출용액매로서 n-헥산과 n-헥산 : 에틸아세테이트(8 : 2)을 사용하여 추출된 부분을 합하여 농축하고 아세톤을 첨가하여 용해된 부분을 추출하고 이 추출 물을 농축시켜 기체 액체 크로마토그래피를 실시하였으며, 전체적인 공정도는 표 1에 나타난 바와 같고 표 2에 분석결과가 나타나 있다.Combine the extracted portions using n-hexane and n-hexane: ethyl acetate (8: 2) as the extraction solution, concentrate, extract the dissolved portion by adding acetone, and concentrate the extract to obtain gas liquid chromatography. The overall process chart is shown in Table 1 and Table 2 shows the analysis results.

[표1]Table 1

분리과정도Separation Process

Figure kpo00002
Figure kpo00002

Figure kpo00003
Figure kpo00003

이와 같은 분리과정에서 사용한 장치 및 조건은 다음과 같다.The apparatus and conditions used in this separation process are as follows.

장 치 : Shimadzu model GC-4BDevice: Shimadzu model GC-4B

검출기 : Hydrogen flame ionization detectorDetector: Hydrogen flame ionization detector

칼 럼 : Shimalite(60-80 mesh) coated 15% BEGS film 2m glass helix shaped tube, 4mm diameter)Column: Shimalite (60-80 mesh) coated 15% BEGS film 2m glass helix shaped tube, 4mm diameter)

칼럼온도 : 130°(150°)-170°(185°)Column Temperature: 130 ° (150 °) -170 ° (185 °)

운반기체 : 질 소Carrier gas: Nitrogen

유 량 : 40ml/minFlow rate: 40ml / min

그리고 기체액체 크로마토그래피 실시전에 백색의 기름상 물질은 얇은막 크로마토그래피 에서는 Rf 0.8이고 BPB가 양성으로 나타났다.Before gas-liquid chromatography, the white oily substance was Rf 0.8 and BPB was positive in thin layer chromatography.

(고정상, 실리카겔 : 전개체, n-헥산 : 에틸아세테이트(8 : 2).(Fixed phase, silica gel: developer, n-hexane: ethyl acetate (8: 2).

또한 적외선 분광측광기에 의하면 1650㎝-1에서 가장 큰 흡수를 나타내었으며, 자외선 분광측광기에 의하면 281nm에서 극내 흡수를 나타내었다.Infrared spectrophotometer showed the largest absorption at 1650cm -1 and ultraviolet spectrophotometer showed in-pole absorption at 281nm.

이상과 같은 분석결과로 마치현(일명 쇠비름)을 특수 처리하여 얻은 항균성물질(유효성분)은 카프로산[CH3(CH2)4COOH], 부티르산[CH3CH2CH2COOH] n-발레르산[CH3CH2CH2COOH] 및 이소발레르산 [(CH3)2CH2CH2COOH]의 네 종류의 지방산임을 확인하였다.As a result of the above analysis, the antimicrobial substance (active ingredient) obtained by special treatment of Machi (aka purslane) was caproic acid [CH 3 (CH 2 ) 4 COOH], butyric acid [CH 3 CH 2 CH 2 COOH] n- valeric acid Four types of fatty acids were identified: [CH 3 CH 2 CH 2 COOH] and isovaleric acid [(CH 3 ) 2 CH 2 CH 2 COOH].

이와같이 하여 얻은 백색의 기름상 물질로 벼의 도열병을 치료한 결과 다음과 같은 결과가 나타났다.The result of treatment of rice blast with rice oil obtained in this way was as follows.

(도열병이 있는 벼를 뽑아 약제처리한 후 26℃의 항온기에서 48시간 습실 처리한 후 현미경으로 조사한 것임)(Paddy rice with blast disease was treated and treated with a microscope after wet treatment in a thermostat at 26 ℃ for 48 hours)

약제 처리별 병반부위포자 잔존량Lesion site spore residual amount by pharmaceutical treatment

Figure kpo00004
Figure kpo00004

비고 : 극소-포자량 100개 이하Remark: Less than 100 micro-spores

소-포자량 100-500개100-500 small spores

중-포자량 500-1000개Medium to spores 500-1000

다-포자량 1000개 이상More than 1000 multi-spores

Claims (5)

마치현을 잘게 분쇄하여 저장탱크에 넣어 발효시킨후 압착하여 농축액을 추출하고, 여기에 메탄올을 첨가하여 용해된 성분을 추출하여 감압 농축하고 여기에 물을 첨가하여 용해된 부분을 염산으로 pH 3.0이 되도록한 후 에틸 아세테이트로 세번 추출하고 감압농축하여, 이 농축액에 n-헥산을 첨가하여 용해된 부분을 추출하여 감압 농축하고 규산 칼럼 크로마토그래피를 실시하고, 추출용매로 n-헥산과 n-헥산 : 에틸(8 : 2)을 사용하여 추출된 부분을 합하여 농축하고 에세톤을 첨가하여 용해된 부분을 추출하고 이 추출물을 능축시켜 기체 액체 크로마토그래피를 실시하는 것을 특징으로 하여 카프로산, 부티르산, n-발레르산 및 이소발레르산으로 된 도열병 치료제의 제조방법.Grind machi finely into a storage tank, fermented and compressed to extract the concentrated solution, methanol is added thereto to extract the dissolved components, concentrated under reduced pressure and water is added thereto to pH 3.0 with hydrochloric acid. The mixture was extracted three times with ethyl acetate, concentrated under reduced pressure, n-hexane was added to the concentrate, the dissolved portion was extracted, concentrated under reduced pressure, silicate column chromatography was carried out, and n-hexane and n-hexane: ethyl were extracted as solvents. Using (8: 2), the extracted portions are combined, concentrated, and extracted by dissolving the added portion by adding acetone. The extract is then subjected to gas liquid chromatography, characterized in that caproic acid, butyric acid, and n-valeric. A method for producing a cure for febrile disease consisting of acid and isovaleric acid. 제1항에 있어서, 저장탱크에서 온도를 35℃-55℃로 하고 24시간마다 교반시키면서 20일간 자연 발효시키는 것을 특징으로 하는 방법.The method of claim 1, wherein the temperature is 35 ℃-55 ℃ in the storage tank, characterized in that the natural fermentation for 20 days with stirring every 24 hours. 제1항 또는 2항에 있어서, 저장탱크에서 100℃ 이상의 수증기로 20-30분간 잘게 분쇄한 마치현을 찌는 것을 특징으로 하는 방법.The method according to claim 1 or 2, characterized in that steaming finely pulverized chopped strings for 20-30 minutes with water vapor of 100 ° C. or higher in a storage tank. 제1항 또는 제2항에 있어서, 저장탱크에서 마치현의 양에 대하여 1/4의 물을 부어 100℃에서 20-30분간 삶는 것을 특징으로 하는 방법.The method according to claim 1 or 2, characterized in that, in a storage tank, pour 1/4 of water with respect to the amount of gusset string and boil at 100 ° C for 20-30 minutes. 제1항에 있어서, 칼럼 충진제를“Wacogel C-200”을 사용하는 것을 특징으로 하는 방법.The method of claim 1, wherein the column filler is used "Wacogel C-200".
KR1019850000709A 1985-02-05 1985-02-05 Preparation of composition for rice-plant fever KR880000348B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101971867A (en) * 2010-10-25 2011-02-16 贵州道元生物技术有限公司 Medicament for treating rice blast
CN106526058A (en) * 2016-11-03 2017-03-22 成都乾坤动物药业股份有限公司 Thin-layer chromatography-fluorescence analysis method for heat-clearing dysentery-stopping granules

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100778107B1 (en) * 2006-07-14 2007-11-29 한국식품연구원 Prepatation method of polysaccharides containing arabinogalactan from portulaca oleracea l

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101971867A (en) * 2010-10-25 2011-02-16 贵州道元生物技术有限公司 Medicament for treating rice blast
CN106526058A (en) * 2016-11-03 2017-03-22 成都乾坤动物药业股份有限公司 Thin-layer chromatography-fluorescence analysis method for heat-clearing dysentery-stopping granules

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