CN111205926A - Ultrahigh pressure extraction method of bupleurum volatile oil - Google Patents

Ultrahigh pressure extraction method of bupleurum volatile oil Download PDF

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Publication number
CN111205926A
CN111205926A CN201811394989.3A CN201811394989A CN111205926A CN 111205926 A CN111205926 A CN 111205926A CN 201811394989 A CN201811394989 A CN 201811394989A CN 111205926 A CN111205926 A CN 111205926A
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volatile oil
solvent
fine powder
pressure
bupleurum
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CN201811394989.3A
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Chinese (zh)
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杨成东
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Nanjing Zelang Medical Technology Co Ltd
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Nanjing Zelang Medical Technology Co Ltd
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Priority to CN201811394989.3A priority Critical patent/CN111205926A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/233Bupleurum
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/37Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Public Health (AREA)
  • Pain & Pain Management (AREA)
  • Rheumatology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Chemical & Material Sciences (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Epidemiology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The application discloses an ultrahigh pressure extraction method of bupleurum volatile oil, which comprises the following steps: step 1, taking a radix bupleuri raw material, crushing the radix bupleuri raw material into fine powder, sieving the fine powder with a 18-mesh sieve, and drying the fine powder for 4 hours at the temperature of 60 ℃; step 2, extracting the bupleurum by using a solvent under the condition of ultrahigh pressure; and 3, separating the solvent and the volatile oil to obtain the volatile oil. The method can efficiently obtain crude volatile oil from bupleuri radix by selecting and controlling extraction solvent, extraction time and extraction pressure, and has the advantages of short extraction time, low energy consumption, low temperature, no thermal damage to active ingredients, etc.

Description

Ultrahigh pressure extraction method of bupleurum volatile oil
Technical Field
The invention belongs to the field of natural product extraction, and relates to an ultrahigh pressure extraction method of bupleurum volatile oil.
Background
Bupleurum root, named as peruvian root, fumigating root, mountain vegetable, taenia herb and bupleurum root. The bupleuri radix is dried root of Bupleurum scorzonerifolium or Bupleurum scorzonerifolium of Umbelliferae. Has the effects of harmonizing shaoyang, soothing liver, resolving stagnation, lifting yang qi and the like, is used for treating diseases such as exogenous fever, stagnation of qi due to depression of the liver, chest and costal pain, sinking of qi due to depression and the like, has been clinically applied for thousands of years in the history of Chinese medicine, and has obvious curative effect. .
The volatile oil is also called essential oil, is a water-immiscible volatile oily component which is obtained in plants by steam distillation and often has specific aromatic odor. In traditional Chinese medicines, many medicinal materials contain volatile oil components and generally have strong pharmacological activity. The bupleurum volatile oil has good antipyretic effect, is complex in volatile oil components, mainly comprises micromolecular aldehydes and esters compounds, monoterpene, sesquiterpene compounds, micromolecular aromatic compounds and the like, has special fragrance, and is active in physicochemical property. Modern pharmaceutical research shows that the volatile oil has small molecular weight, strong lipid solubility, high bioavailability, rapid absorption and action, and is easy to penetrate in vivo biological membrane, and is consistent with the theory of traditional Chinese medicine.
At present, the extraction method of the volatile oil mainly comprises a steam distillation method, a grease absorption method, a solvent extraction method, a supercritical fluid extraction method, a cold pressing method and the like for extraction, wherein the most common method is the steam distillation method, but when the method is used for further separation and refining, the traditional redistillation method has the defects that the volatile oil is easy to oxidize and deteriorate and the yield is low due to longer heating times and time. The supercritical CO2 extraction of the volatile oil has higher yield, but the cost of investment in industrial production amplification is high. Therefore, how to obtain more volatile oil components becomes a problem.
The ultrahigh pressure is called as ultrahigh cold isostatic pressing, and is called as cold isostatic pressing for short, and the ultrahigh pressure is the hydrostatic pressure with the pressure of 100-1000 MPa. The ultrahigh pressure biological treatment technology has wide application field, and provides a new platform for scientific research, product development and process innovation of biological, medical and food engineering. Based on the new technology, the traditional Chinese medicine extraction field has literature reports: compared with the traditional extraction technology, the ultrahigh pressure extraction technology can greatly shorten the extraction time, reduce the energy consumption, reduce the dissolution of impurity components, improve the yield of effective components and the like, so the research of the ultrahigh pressure extraction technology is proposed to improve the extraction efficiency.
Disclosure of Invention
The invention aims to provide a method for efficiently extracting crude bupleurum essential oil, provides an efficient and convenient technical means for obtaining the bupleurum essential oil, and realizes the effects of energy conservation and efficient utilization of resources.
The method comprises the following steps:
step 1, taking a radix bupleuri raw material, crushing the radix bupleuri raw material into fine powder, sieving the fine powder with a 18-mesh sieve, and drying the fine powder for 4 hours at the temperature of 60 ℃;
step 2, extracting the bupleurum by using a solvent under the condition of ultrahigh pressure;
step 3, separating the solvent and the volatile oil to obtain the volatile oil;
wherein, the solvent in step 2 is selected from any solvent capable of dissolving the volatile oil of the traditional Chinese medicine, including but not limited to ethanol, methanol, diethyl ether, carbon disulfide, chloroform, ethyl acetate, n-butanol, petroleum ether, n-hexane, and their mixture and their aqueous solution; the dosage of the solvent is 1-60 times of the volume of the weight of the traditional Chinese medicinal materials; the ultrahigh pressure condition is that the pressure range is required to be controlled to be 100-1000Mpa during extraction; the duration of the ultrahigh pressure extraction is 1-30 minutes;
wherein, the solvent and the volatile oil are separated in the step 3 by adopting a normal pressure or reduced pressure distillation method.
Example (b):
example 1
Taking 20g of radix bupleuri medicinal material, adding 200ml of 95% ethanol, extracting for 10min under the condition of 400Mpa ultrahigh pressure, filtering to obtain an extracting solution, recovering ethanol from the extracting solution at 60 ℃ under reduced pressure to obtain crude volatile oil, wherein the crude volatile oil is 2.43g of radix bupleuri crude oil through detection, and the yield is 12.15%.
Example 2
Collecting bupleuri radix 20g, adding 1200ml 40% ethanol, extracting under 1000Mpa ultra-high pressure for 5min, filtering to obtain extractive solution, recovering ethanol from the extractive solution at 40 deg.C under reduced pressure to obtain crude volatile oil 2.06g with yield of 10.3%.
Example 3
Taking 20g of radix bupleuri medicinal material, adding 60ml of absolute ethanol, extracting for 30min under the condition of 100Mpa ultrahigh pressure, filtering to obtain an extracting solution, and recovering ethanol from the extracting solution at 90 ℃ under reduced pressure to obtain 2.23g of crude volatile oil with the yield of 11.15%.
Example 4
Collecting bupleuri radix 200g, adding 1000ml 95% ethanol, extracting under 200Mpa and ultrahigh pressure for 5min, filtering to obtain extractive solution, recovering ethanol from the extractive solution at 30 deg.C under reduced pressure to obtain crude volatile oil 18.76g with yield of 9.38%.
Example 5
Collecting bupleuri radix 200g, adding 5000ml 80% ethanol, extracting under 800Mpa ultra-high pressure for 30min, filtering to obtain extractive solution, recovering ethanol from the extractive solution at 40 deg.C under reduced pressure to obtain crude volatile oil 20.83g with yield of 10.42%.

Claims (4)

1. A method for efficiently extracting crude volatile oil is characterized by comprising the following steps:
step 1, taking a radix bupleuri raw material, crushing the radix bupleuri raw material into fine powder, sieving the fine powder with a 18-mesh sieve, and drying the fine powder for 4 hours at the temperature of 60 ℃;
step 2, extracting the bupleurum by using a solvent under the condition of ultrahigh pressure;
step 3, separating the solvent and the volatile oil to obtain the volatile oil;
wherein, the solvent in step 2 is selected from any solvent capable of dissolving the volatile oil of the traditional Chinese medicine, including but not limited to ethanol, methanol, diethyl ether, carbon disulfide, chloroform, ethyl acetate, n-butanol, petroleum ether, n-hexane, and their mixture and their aqueous solution.
Wherein, the solvent and the volatile oil are separated in the step 3 by adopting a normal pressure or reduced pressure distillation method.
2. The method according to claim 1, wherein the solvent used in step 2 is 1 to 60 times by volume of the solvent.
3. The process of claim 1, wherein the ultra-high pressure conditions in step 2 are: the pressure is 100-1000Mpa, and the extraction time is 5-30 min.
4. The method of claim 1, wherein the step 3 comprises filtering to obtain an extract, and distilling the extract at 40-90 deg.C under reduced pressure to obtain the volatile oil.
CN201811394989.3A 2018-11-22 2018-11-22 Ultrahigh pressure extraction method of bupleurum volatile oil Pending CN111205926A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811394989.3A CN111205926A (en) 2018-11-22 2018-11-22 Ultrahigh pressure extraction method of bupleurum volatile oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114561245A (en) * 2022-02-14 2022-05-31 中国人民解放军海军军医大学 Method for simultaneously distilling and extracting bupleurum volatile oil

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114561245A (en) * 2022-02-14 2022-05-31 中国人民解放军海军军医大学 Method for simultaneously distilling and extracting bupleurum volatile oil

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