CN104382978A - Method for extracting effective components of leaves of honeysuckle - Google Patents

Method for extracting effective components of leaves of honeysuckle Download PDF

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Publication number
CN104382978A
CN104382978A CN201410592734.3A CN201410592734A CN104382978A CN 104382978 A CN104382978 A CN 104382978A CN 201410592734 A CN201410592734 A CN 201410592734A CN 104382978 A CN104382978 A CN 104382978A
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CN
China
Prior art keywords
extraction
leaf
flos lonicerae
entrainer
separating still
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410592734.3A
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Chinese (zh)
Inventor
李洪哲
袁煜昊
杨宏书
于素雷
李晓燕
李淼
叶春
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GUANGXI JINHAO BIO-TECHNOLOGY Co Ltd
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GUANGXI JINHAO BIO-TECHNOLOGY Co Ltd
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Priority to CN201410592734.3A priority Critical patent/CN104382978A/en
Publication of CN104382978A publication Critical patent/CN104382978A/en
Pending legal-status Critical Current

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    • 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)
    • A61K36/35—Caprifoliaceae (Honeysuckle family)
    • A61K36/355—Lonicera (honeysuckle)
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a method for extracting effective components of leaves of honeysuckle. The method comprises the following steps: (1) preprocessing leaves of honeysuckle; (2) putting powder obtained in the step (1) into an extraction kettle of a supercritical CO2 extraction device, adding an ultrasonic generator, adding an entrainer and then extracting; and (3) removing the entrainer by reduced pressure distillation, discharging from a separation kettle, and then obtaining an extract of the leaves of honeysuckle in a spray drying manner. The method is simple in process and easy to operate; the content of the extract is high; due to adoption of flower buds and stems and leaves of the honeysuckle as raw materials, the application value of a honeysuckle plant is effectively expanded; and resource waste is avoided.

Description

A kind of extracting method of leaf of Flos Lonicerae effective ingredient
Technical field
The present invention relates to field of medicaments, specifically, is a kind of extracting method of leaf of Flos Lonicerae effective ingredient.
Background technology
Flos Lonicerae (Lonicera japonica) is for Caprifoliaceae woodbine Radix Ophiopogonis and congener dry flower or be with the flower just opened, and is one of clinical conventional Chinese crude drug, has effect of heat-clearing and toxic substances removing, dispelling wind and heat pathogens.The effective ingredient of Flos Lonicerae is chlorogenic acid, isochlorogenic acid, and flavonoid and volatilization wet goods, wherein, chlorogenic acid has antibacterial, antiviral, increases the effects such as leukocyte, hepatic cholagogic, antitumor, blood pressure lowering, blood fat reducing, scavenging free radicals and stimulating central nervous system system.
The traditional method extracting Flos Lonicerae is only raw material with Lonicera japonica, mainly contains water extraction, ethanol refluxing process, decoction and alcohol sedimentation technique, enzymatic isolation method etc., all there is length consuming time, power consumption is large, product purity is low, processing cost crosses the problems such as high.
Summary of the invention
Technical problem to be solved by this invention is the defect overcoming prior art, provides a kind of extracting method of leaf of Flos Lonicerae effective ingredient, the method technique is simple, easy to operate, extractive content is high.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of extracting method of leaf of Flos Lonicerae effective ingredient, comprises following processing step:
(1) pretreatment: leaf of Flos Lonicerae is cleaned and drains, dry, be ground into 20 ~ 40 object powder;
(2) ultrasonic assistant supercritical CO 2extraction: step (1) gained powder is inserted supercritical CO 2in the extraction kettle of extraction equipment, install ultrasonic generator additional, and add entrainer, then extract, wherein supercritical CO 2extraction conditions is: extraction kettle pressure 20 ~ 40MPa, temperature 35 ~ 50 DEG C, separating still I pressure 10 ~ 20MPa, temperature 20 ~ 30 DEG C, separating still II pressure 5 ~ 10MPa, temperature 30 ~ 45 DEG C, CO 2circular flow 5 ~ 10kg/h, extraction time 1 ~ 3 hour; Ultrasonic assistant extraction conditions is: supersonic frequency 20 ~ 100KHz, ultrasonic power density 20 ~ 100W/L;
(3) through distilling under reduced pressure, entrainer is removed, from separating still I and separating still II discharging, more spray-dried, the extract of leaf of Flos Lonicerae can be obtained.
In described step (1), drying condition is: temperature 30 ~ 40 DEG C, 18 ~ 24 hours time.
In described step (2), entrainer is specially: 95% ethanol, 3 ~ 5 times that the amount that entrainer adds is added powder quality.
In described step (2), supercritical CO 2fluid extraction route: CO 2steel cylinder → refrigeration system → high-pressure pump → extraction kettle → separating still I → separating still II → basin → circulation.
The extracting method of above-mentioned leaf of Flos Lonicerae effective ingredient, can simplified summary be: leaf of Flos Lonicerae → pretreatment → ultrasonic assistant supercritical CO 2extract → remove entrainer → separating still discharging → spraying dry → effective ingredient of honeysuckle.
The invention has the beneficial effects as follows:
1, the present invention is by ultrasonic extraction and supercritical CO 2extraction phase combines, and improves original simple supercritical CO 2extraction efficiency, and method is simple, efficient, safety.
2, the present invention utilizes the alabastrum of Flos Lonicerae and stem and leaf to be raw material effective component extracting, changes the way of traditional simple effective component extracting from Lonicera japonica, has effectively expanded the using value of Flos Lonicerae plant, avoided the wasting of resources.
3, the present invention extracts overall process is all carry out below 50 DEG C, can prevent the oxidation of leaf of Flos Lonicerae Content of Chlorogenic Acid, separation.
Detailed description of the invention
Be described principle of the present invention and feature below in conjunction with specific embodiment, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1:
An extracting method for leaf of Flos Lonicerae effective ingredient, comprises following processing step:
(1) pretreatment: by leaf of Flos Lonicerae clean drain, at 20 DEG C dry 24 hours, be ground into 40 object powder;
(2) ultrasonic assistant supercritical CO 2extraction: step (1) gained powder is loaded supercritical CO 2in the extraction kettle of extraction equipment, install ultrasonic generator additional, and to add 95% ethanol be entrainer, 3 times that the amount that entrainer adds is added powder quality, then extract, setting extraction kettle pressure 20MPa, temperature 35 DEG C, separating still I pressure 10MPa, temperature 20 DEG C, separating still II pressure 5MPa, temperature 30 DEG C, CO 2circular flow 5kg/h, extraction time 3 hours; Ultrasonic assistant extraction conditions is: supersonic frequency 100KHz, ultrasonic power density 100W/L;
(3) through distilling under reduced pressure, entrainer is removed, from separating still I and separating still II discharging, more spray-dried, the extract of leaf of Flos Lonicerae can be obtained.
Embodiment 2:
An extracting method for leaf of Flos Lonicerae effective ingredient, comprises following processing step:
(1) pretreatment: leaf of Flos Lonicerae is cleaned and drains, lower oven dry 20 hours at 30 DEG C, be ground into 30 object powder;
(2) ultrasonic assistant supercritical CO 2extraction: step (1) gained powder is loaded supercritical CO 2in the extraction kettle of extraction equipment, install ultrasonic generator additional, and to add 95% ethanol be entrainer, 4 times that the amount that entrainer adds is added powder quality, then extract, setting extraction kettle pressure 30MPa, temperature 35 DEG C, separating still I pressure 15MPa, temperature 25 DEG C, separating still II pressure 8MPa, temperature 40 DEG C, CO 2circular flow 8kg/h, extraction time 2 hours; Ultrasonic assistant extraction conditions is: supersonic frequency 50KHz, ultrasonic power density 50W/L;
(3) through distilling under reduced pressure, entrainer is removed, from separating still I and separating still II discharging, more spray-dried, the extract of leaf of Flos Lonicerae can be obtained.
Embodiment 3:
An extracting method for leaf of Flos Lonicerae effective ingredient, comprises following processing step:
(1) pretreatment: leaf of Flos Lonicerae is cleaned and drains, lower oven dry 18 hours at 40 DEG C, be ground into 20 object powder;
(2) ultrasonic assistant supercritical CO 2extraction: step (1) gained powder is loaded supercritical CO 2in the extraction kettle of extraction equipment, install ultrasonic generator additional, and to add 95% ethanol be entrainer, 5 times that the amount that entrainer adds is added powder quality, then extract, setting extraction kettle pressure 40MPa, temperature 50 C, separating still I pressure 20MPa, temperature 30 DEG C, separating still II pressure 10MPa, temperature 45 C, CO 2circular flow 10kg/h, extraction time 1 hour; Ultrasonic assistant extraction conditions is: supersonic frequency 10KHz, ultrasonic power density 20W/L;
(3) through distilling under reduced pressure, entrainer is removed, from separating still I and separating still II discharging, more spray-dried, the extract of leaf of Flos Lonicerae can be obtained.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. an extracting method for leaf of Flos Lonicerae effective ingredient, is characterized in that: comprise following processing step:
(1) pretreatment: leaf of Flos Lonicerae is cleaned and drains, dry, be ground into 20 ~ 40 object powder;
(2) ultrasonic assistant supercritical CO 2extraction: step (1) gained powder is inserted supercritical CO 2in the extraction kettle of extraction equipment, install ultrasonic generator additional, and add entrainer, then extract, wherein supercritical CO 2extraction conditions is: extraction kettle pressure 20 ~ 40MPa, temperature 35 ~ 50 DEG C, separating still I pressure 10 ~ 20MPa, temperature 20 ~ 30 DEG C, separating still II pressure 5 ~ 10MPa, temperature 30 ~ 45 DEG C, CO 2circular flow 5 ~ 10kg/h, extraction time 1 ~ 3 hour; Ultrasonic assistant extraction conditions is: supersonic frequency 20 ~ 100KHz, ultrasonic power density 20 ~ 100W/L;
(3) through distilling under reduced pressure, entrainer is removed, from separating still I and separating still II discharging, more spray-dried, the extract of leaf of Flos Lonicerae can be obtained.
2. the extracting method of a kind of leaf of Flos Lonicerae effective ingredient according to claim 1, is characterized in that: in described step (1), drying condition is: temperature 30 ~ 40 DEG C, 18 ~ 24 hours time.
3. the extracting method of a kind of leaf of Flos Lonicerae effective ingredient according to claim 1, it is characterized in that: in described step (2), entrainer is 95% ethanol, 3 ~ 5 times that the amount that entrainer adds is added powder quality.
CN201410592734.3A 2014-10-28 2014-10-28 Method for extracting effective components of leaves of honeysuckle Pending CN104382978A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105535834A (en) * 2016-01-05 2016-05-04 陈杏芬 Traditional Chinese medicine preparation for treating hand-foot-and-mouth disease and preparation method and application thereof
CN111249325A (en) * 2020-03-19 2020-06-09 山东华夏高科农业科技发展有限公司 Method for collecting honeysuckle cell sap

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002060379A2 (en) * 2000-10-25 2002-08-08 National Engineering Research Center For Traditional Chinese Medicine Composition comprising extracts of flos lonicerae, fructus forsythiae and radix scutellariae, uses and preparation thereof
CN102166249A (en) * 2011-03-11 2011-08-31 河北科星药业有限公司 Method for extracting active ingredients from honeysuckle leaves
CN102676290A (en) * 2012-04-27 2012-09-19 无限极（中国）有限公司 Ultrasonic assisted supercritical CO2 hemp seed oil extraction method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002060379A2 (en) * 2000-10-25 2002-08-08 National Engineering Research Center For Traditional Chinese Medicine Composition comprising extracts of flos lonicerae, fructus forsythiae and radix scutellariae, uses and preparation thereof
WO2002060379A3 (en) * 2000-10-25 2003-03-13 Nat Engineering Res Ct For Tra Composition comprising extracts of flos lonicerae, fructus forsythiae and radix scutellariae, uses and preparation thereof
CN102166249A (en) * 2011-03-11 2011-08-31 河北科星药业有限公司 Method for extracting active ingredients from honeysuckle leaves
CN102676290A (en) * 2012-04-27 2012-09-19 无限极（中国）有限公司 Ultrasonic assisted supercritical CO2 hemp seed oil extraction method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
钟玲等: "超临界CO2萃取金银花叶中绿原酸及挥发油成分研究", 《亚太传统医药》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105535834A (en) * 2016-01-05 2016-05-04 陈杏芬 Traditional Chinese medicine preparation for treating hand-foot-and-mouth disease and preparation method and application thereof
CN111249325A (en) * 2020-03-19 2020-06-09 山东华夏高科农业科技发展有限公司 Method for collecting honeysuckle cell sap

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