KR100764610B1 - The Natural Product Extractor and Method by Vacuum and High Pressure Impulse - Google Patents
The Natural Product Extractor and Method by Vacuum and High Pressure Impulse Download PDFInfo
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- 229930014626 natural product Natural products 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 22
- 239000000284 extract Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims description 12
- 230000035939 shock Effects 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000004899 motility Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 210000002615 epidermis Anatomy 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 241000208340 Araliaceae Species 0.000 description 5
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 5
- 235000003140 Panax quinquefolius Nutrition 0.000 description 5
- 235000008434 ginseng Nutrition 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 2
- 229930182490 saponin Natural products 0.000 description 2
- 150000007949 saponins Chemical class 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 235000002789 Panax ginseng Nutrition 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- 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
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- 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
- A23V2250/00—Food ingredients
- A23V2250/20—Natural extracts
- A23V2250/21—Plant extracts
- A23V2250/2124—Ginseng
-
- 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
- A23V2300/00—Processes
- A23V2300/14—Extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Botany (AREA)
- Mycology (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Epidemiology (AREA)
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- Extraction Or Liquid Replacement (AREA)
Abstract
본 발명은 천연물의 추출 방법 및 장치에 관한 것으로, 천연물의 활성물질이 분해되지 않는 최대 허용 온도 이하에서, 급속 진공 및 가압으로 천연물 내의 모세관을 통로로 하여 추출액을 이동시킴으로써, 기존의 방법에서 추출하려는 물질이 표피층으로 이동하는 데 걸리는 시간을 단축하고, 저온에서 가능케 함으로써 유용물질을 분해 없이 효율적으로 추출하는 방법 및 장치이다.The present invention relates to a method and apparatus for extracting a natural product, wherein the extract is moved through a capillary tube in the natural product by rapid vacuum and pressure at a maximum allowable temperature at which the active substance of the natural product does not decompose, thereby extracting the conventional method A method and apparatus for efficiently extracting useful materials without degradation by shortening the time taken for the material to move to the epidermal layer and enabling it at low temperatures.
진공, 가압, 충격, 저온, 천연물 추출, 추출액, 활성물질Vacuum, pressurization, impact, low temperature, natural product extraction, extract, active substance
Description
도 1은 본 발명의 방법에 사용되는 장치를 보여 주는 모식도.1 is a schematic diagram showing an apparatus used in the method of the present invention.
도 2는 인삼을 시료로 하는 추출 수율에 있어서, 추출 조건별로 영향을 보여주는 그래프.Figure 2 is a graph showing the influence of the extraction conditions in the extraction yield using ginseng as a sample.
<도면의 주요부분에 대한 부호의 설명><Description of the code | symbol about the principal part of drawing>
1. 추출기 1a. 원료용기1.
2. 용매 저장기 3. 증기응축 진공탱크2. Solvent
4. 가압 탱크 5. 응축기4. Pressurized
6. 응축수 수집기 7. 농축기6. Condensate Collector 7. Thickener
8. 히터 9. 진공계8. Heater 9. Vacuum meter
10a, 10b. 건조증기밸브 11, 11a, 11b. 밸브10a, 10b.
12. 밸브 13. 열전달 매체용 펌프12. Valve 13. Pump for Heat Transfer Media
14. 진공 라인 15. 냉각수 라인14.
16. 가열 라인16. heating line
본 발명은 식품 및 의약품 산업 분야에 사용될 수 있는 식물성 천연물 원료의 추출 방법 및 장치에 관한 것으로, 상세하게는, 식물성 천연물 원료의 추출 공정에서 열 및 가수분해에 민감한 유용성분의 활성이 유지되는 상태에서 추출 효율을 극대화시킬 수 있는 추출 방법 및 이에 사용되는 장치에 관한 것이다.The present invention relates to a method and apparatus for extracting vegetable natural raw materials that can be used in the food and pharmaceutical industry, and more particularly, in the state of maintaining the activity of useful components sensitive to heat and hydrolysis in the extraction process of vegetable natural raw materials. The present invention relates to an extraction method for maximizing extraction efficiency and an apparatus used therefor.
종래에는 분해를 억제하기 위하여 유기용매를 사용하고 추출 후 이 용매를 제거하는 공정이 필요하였고, 유기용매로 인한 화재의 위험이 있었다. 유기용매를 쓰지 않는 고온 열탕 방법의 추출 공정은 유효성분의 열분해가 심하게 일어나고, 막대한 시간의 소요되었으며 추출 수율이 낮았다.Conventionally, in order to suppress decomposition, a process of using an organic solvent and removing the solvent after extraction was required, and there was a risk of fire due to the organic solvent. The extraction process of the hot boiling water method using no organic solvent was severely thermally decomposed of the active ingredient, required a great time, and the extraction yield was low.
따라서 본 발명의 목적은 의약 및 식품 산업에서 사용되는 식물성 천연물 원료의 추출 시간을 단축시키고, 활성이 있는 유용한 성분, 특히 열에 민감한 성분의 생물학적 활성을 유지하면서 단 시간 내에 최대의 추출 효과를 얻을 수 있는 추출방법을 제공하고자 하는 것이다Therefore, an object of the present invention is to shorten the extraction time of the plant natural product raw materials used in the pharmaceutical and food industry, and to obtain the maximum extraction effect in a short time while maintaining the biological activity of active useful components, especially heat sensitive components. To provide an extraction method.
상기 목적을 달성하기 위하여 본 발명은 일반적인 진공 추출장치에 저렴한 비용으로 대용량의 진공을 제공하는 증기응축진공탱크, 상기의 진공탱크로부터 추출기 내부를 급속히 진공상태로 만들 수 있는 신속 작용 밸브, 추출기 내부의 진공상태를 급속히 고압 상태로 만들어 줄 수 있는 가압탱크가 부가적으로 필요하다.In order to achieve the above object, the present invention provides a condensation vacuum tank for providing a large-capacity vacuum at a low cost to a general vacuum extraction device, a quick action valve which can rapidly make the inside of the extractor from the vacuum tank, the inside of the extractor. There is additionally a need for a pressurized tank that can rapidly bring the vacuum to high pressure.
더욱 상세하게는 진공탱크가 1㎜Hg 이하의 진공 상태에서도 원형이 유지될 수 있게 되어야 하며, 신속 작용 밸브는 0.05초 이내에 개폐가 가능한 밸브로 사용하여야 하고, 가압탱크는 10기압 정도를 제공할 수 있는 것이면 된다.More specifically, the vacuum tank should be able to maintain a circular shape even under vacuum of 1 mmHg or less, the quick acting valve should be used as a valve that can be opened and closed within 0.05 seconds, the pressure tank can provide about 10 atm. You just need to be.
실시예Example
1) 재료1) material
본 실험에 재료로 쓰인 인삼은 6년근 수삼을 홍삼으로 제조하여 동체와 미삼을 2:1의 비율로 혼합하여 사용하였다.The ginseng used as a material for this experiment was prepared by using
2) 추출2) extraction
인삼 분말을 도 1에 나타낸 장치를 사용하여 본 발명에 따른 진공-가압 충격의 추출 방법을 실시하였다.Ginseng powder was subjected to the vacuum-pressure shock extraction method according to the present invention using the apparatus shown in FIG. 1.
인삼 분말을 추출기(1)에 700g를 넣고 용매 저장기(2)에는 증류수를 2/3 정도까지 유입시킨 후, 히터(8)를 작동시켜 용매 저장기(2) 및 추출기(1)의 내용물을 30∼55℃ 까지 가열하였다. 추출기(1)에서 진공탱크와 연결된 신속 작용 밸브(11)를 조절하여 잔류압력 5 ㎜Hg 이하까지 0.1 초 동안 진공-펄스 처리하고 10 분 동안 진공 하에서 유지시킨 후, 신속 작용밸브(11)를 폐쇄하고 가압탱크(4)와 연결된 밸브(11a)를 개방하여 0.1 초 동안에 가압 상태로 바꾸는 조작을 4 회 반복하였다.700 g of ginseng powder was added to the extractor (1), distilled water was introduced into the solvent reservoir (2) to about 2/3, and the heater (8) was operated to remove the contents of the solvent reservoir (2) and the extractor (1). It heated to 30-55 degreeC. In the extractor 1, the
용매 내의 탈기(脫氣)를 위하여 상기와 같은 방법으로 용매 저장기(2)에 대하여도 동일하게 적용하였으며 단지 진공을 해제할 때 신속 작용 밸브(11b)는 가압탱크 대신에 대기와 연결 시켰다.The same applies to the
예비 작업이 끝나면, 용매 저장기(2)와 추출기(1) 사이에 연결된 밸브(13)을 개방하여 추출기(1)에 증류수를 채웠다. 곧 이어 추출기(1) 내 상부의 공기가 증류 수내에 용해될 시간적 간격을 두지 않고 곧 바로 추출기(1)에 대하여 예비 작업과 같은 방법을 7회 반복 조작하였다.After the preliminary work, the valve 13 connected between the
3) 사포닌 정량 및 분해 패턴 분석3) Saponin quantification and degradation pattern analysis
眞空 및 力積壓縮方式으로 추출·농축된 엑스를 수포화 n-butanol 추출법으로 조사포닌을 추출 분리하여 메탄올에 용해시켜 고속 액체크로마토그래피로 분석하였다.Extracted and concentrated extracts were extracted and concentrated by distillation and distillation, and then extracted by distillation of irradiated n-butanol, dissolved in methanol, and analyzed by high performance liquid chromatography.
고속 액체크로마토그래피 분석 조건은 LiChrosorb-NH2 column(Φ 4.6 ㎜ I.D × 250 ㎜, 10 ㎛)에 이동상으로 acetonitrile/water/n-butanol(80/20/10, v/v)을 사용하고 유속은 1.0 ㎖/min으로 하여 굴절검출기(RI)로 검출 정량하였다. 사포닌 분해형태 및 분석을 위하여 고속 액체크로마토그래피로 역상( Waters, 3.9 × 150 ㎜) 칼럼을 사용하고, 이동상 용매는 기울기 용리를 사용하여 전개시켰다.High-speed liquid chromatography analysis conditions use acetonitrile / water / n-butanol (80/20/10, v / v) as a mobile phase on a LiChrosorb-NH 2 column (Φ 4.6 mm ID × 250 mm, 10 μm). Detection was quantified by a refraction detector (RI) at 1.0 ml / min. Reversed phase with high-performance liquid chromatography for saponin degradation forms and analysis Waters, 3.9 × 150 mm) column, and mobile phase solvent was developed using gradient elution.
4) 품질 및 관능 조사4) Quality and sensory investigation
색도 측정은 Minolta chronometer CR-200을 사용하였고, 갈색도는 UV-Vis Scanning spectrophotometer(UV-2101PC Shimadzu Co.)를 사용하여 440 nm에서 측정하였다. 점도는 평판 점도계(Sanyo Co., LTD.)를 사용하여 측정하였으며 같은 含水分에서 시험하였다.The chromaticity was measured using a Minolta chronometer CR-200, and the brownness was measured at 440 nm using a UV-Vis Scanning spectrophotometer (UV-2101PC Shimadzu Co.). Viscosity was measured using a plate viscometer (Sanyo Co., LTD.) And tested at the same water content.
향미 관능 검사는 14명의 panel이 향미묘사법(flavor profile method)에 의하여 각 1.0 g씩 냉수 100 ㎖을 가하여 충분히 저어준 다음 향미평가를 실시하였는 데, 냄새를 맡는 방법은 컵을 흔들어 냄새 성분이 잘 휘발되도록 하여 빠르게 흡입하게 하고, 맛은 시료를 입안에 넣어 혀의 전면에 고루 묻혀서 시료의 맛과 향에 대하여 9단계의 기호척도법으로 강도를 표시하게 하여 이를 quantitative descriptive analysis (QDA)방법으로 표시하였다.The taste sensory test was carried out by 14 panelists after adding 100 ml of cold water at 1.0 g each by flavor profile method. After stirring, the evaluation of the taste was carried out. Inhaled quickly by volatilization, the taste was embedded in the mouth and spread evenly over the front of the tongue, indicating the intensity and taste of the sample by nine-step symbolic scale, which was expressed by quantitative descriptive analysis (QDA). .
비교예 1Comparative Example 1
실시예의 추출기(1) 및 원료 용기(1a)를 사용하여 80℃ 열탕으로 추출하였다.It extracted with 80 degreeC hot water using the extractor 1 of the Example, and the
비교예 2Comparative Example 2
실시예의 장치에서 추출기(1)의 진공 상태를 해제할 때 가압탱크(4) 대신에 대기와 연결하여 대기압의 상태를 유지하였다.When releasing the vacuum state of the extractor 1 in the apparatus of the embodiment, the state of atmospheric pressure was maintained by connecting with the atmosphere instead of the
도 2에서 보듯이, 본 발명에 따른 방법을 사용하면 대기압 고온 추출 또는 진공-대기압 추출의 경우보다 추출 수율이 높을 뿐 아니라, 추출에 소요되는 시간이 경제적으로 단축된다는 것을 알 수 있다.As shown in FIG. 2, it can be seen that the use of the method according to the invention not only results in higher extraction yields than in the case of atmospheric hot extraction or vacuum-atmospheric extraction, but also economically shortens the time required for extraction.
이상의 결과에서와 같이, 본 발명은 진공 및 가압시 원료 내부 모세관 통로에서 추출액의 운동성을 크게 하여 추출 수율을 높이고 또한 낮은 온도에서 식물성 천연물을 추출할 수 있어 인체에 유용한 활성 성분이 감소되지 않아서 추출물의 효능 및 부가가치를 한층 더 높힐 수 있다.As described above, the present invention can increase the extraction yield by increasing the motility of the extract in the capillary passage inside the raw material during vacuum and pressurization, and also can extract the plant natural product at low temperature, so that the active ingredient useful for the human body is not reduced. Efficacy and added value can be further increased.
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KR101404618B1 (en) * | 2012-08-10 | 2014-06-09 | 주식회사 영일이엔지 | Vacuum low temperature extraction apparatus for producing indigo pigment |
US11612558B2 (en) * | 2019-06-03 | 2023-03-28 | Ping Li | Methods of extracting materials from plant material |
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KR960030943A (en) * | 1995-02-23 | 1996-09-17 | 최진태 | Method of manufacturing pine needle extract |
JPH09169980A (en) * | 1995-12-19 | 1997-06-30 | Hisaka Works Ltd | Extraction from wood and device used therefor |
KR970074911A (en) * | 1996-05-13 | 1997-12-10 | 롤란드 엠 허버트 | Oil extraction method from oil-containing plants |
KR20020046394A (en) * | 2000-12-13 | 2002-06-21 | 윤승열 | Extraction Apparatus Method For Essential terpene-oil |
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KR960030943A (en) * | 1995-02-23 | 1996-09-17 | 최진태 | Method of manufacturing pine needle extract |
JPH09169980A (en) * | 1995-12-19 | 1997-06-30 | Hisaka Works Ltd | Extraction from wood and device used therefor |
KR970074911A (en) * | 1996-05-13 | 1997-12-10 | 롤란드 엠 허버트 | Oil extraction method from oil-containing plants |
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