CN106265852A - The method of bioactive ingredients in Cuculus polioephalus is spent in a kind of extraction in vain - Google Patents

The method of bioactive ingredients in Cuculus polioephalus is spent in a kind of extraction in vain Download PDF

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Publication number
CN106265852A
CN106265852A CN201610848272.6A CN201610848272A CN106265852A CN 106265852 A CN106265852 A CN 106265852A CN 201610848272 A CN201610848272 A CN 201610848272A CN 106265852 A CN106265852 A CN 106265852A
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China
Prior art keywords
extraction
vain
cuculus polioephalus
florescence
spending
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Pending
Application number
CN201610848272.6A
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Chinese (zh)
Inventor
郝宝成
班旦
拉巴次旦
刘宇
梁剑平
陶蕾
王学红
尚若锋
郭文柱
杨珍
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Lanzhou Institute of Animal Husbandry and Veterinary Medicine CAAS
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Lanzhou Institute of Animal Husbandry and Veterinary Medicine CAAS
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Priority to CN201610848272.6A priority Critical patent/CN106265852A/en
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    • 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)
    • A61K36/45Ericaceae or Vacciniaceae (Heath or Blueberry family), e.g. blueberry, cranberry or bilberry
    • 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

Abstract

The present invention provides a kind of extraction to spend the method for bioactive ingredients in Cuculus polioephalus in vain, and spending in vain after Cuculus polioephalus is pulverized of being plucked florescence is put in extraction kettle, with CO2Fluid is extractant, and extracting pressure 15 25MPa, extraction temperature are 35 45 DEG C, extraction time is 1.5 2.5h, obtain the extract of flaxen active component.In the process parameters range that the present invention provides, spending bioactive ingredients extraction efficiency height in Folium Rhododendri Simsii in vain for pluck florescence, extraction rate is fast, technique is simple, saves reagent, and power consumption is few, low cost, pollutes few, is better than other extracting method using traditional extraction technology.

Description

The method of bioactive ingredients in Cuculus polioephalus is spent in a kind of extraction in vain
Technical field
The invention belongs to Separation of Natural Products technical field, be specifically related to a kind of extraction and spend the side of active component in Cuculus polioephalus in vain Method.
Background technology
Rhododendron in Lushan Botanical Garden chemistry is mainly composed of Chenopodium Oil Chenopodium Oil plain, different element, Quercetin, kaempferide, Radix Hyperici Monogyni (Herba Hyperici Monogyni) Glycoside, red pigment, sitosterol etc..Ericad active component has good antibacterial and anti-inflammation functions, such as beautiful Cuculus polioephalus, Wenchuan Du Cuckoo, the antibacterial action of short Folium Eriobotryae are just better than or are equivalent to Rhizoma Coptidis.But in recent years, it is more subject to weight as neuro pharmacology substrate Depending on.
The chemical composition that James A.Klock etc. extract from Azalea pontica is as the treatment of cardiovascular drug;Yoshiki etc. from Extracting 2 kinds of new chromanane derivants 1 and chromanane derivant 2 in Folium Cuculus polioephalus, another kind of compound chromogen alkene 3 has Potential anti-hiv activity;Zhong Guohua etc., using Azalea pontica as anesthetis, treat pyrexial malaria, have significant decreased heart rate and The effect of reducing blood pressure.The farrerol separated from magnificent rhododendron leaves and Matleucinal can affect vision.The tender leaf of Rhododendron simsii Planch. is The main component of " heart mixture ", has good efficacy, Folium Rhododendri Daurici, Folium et Cacumen Rhododendri Mariae to have the merit of relieving cough and resolving phlegm to chronic bronchitis Effect.The Diterpenes Diterpenoids,grayanotoxins. of isolated from sweetshell rhododendron leaf leafObvious blood pressure lowering is had to make when low dosage (1~100 μ g/kg) With, moreover it is possible to the induction nervus centripetalis of animal, vagus nerve, muscular nerve, cervical nerves, carotid nerve and Cortical neurons produce strong Burst effect, it was demonstrated that be the flesh analeptic of a kind of high intensity.
It addition, preventing and treating subterranean pest-insect, impregnation process are executed in Azalea pontica medicine liquid spray preventing and treating mulberry yellow moth, filling in ericad Aphid is respond well, and stifling housefly, lethal time is identical with perian insect powder, and recovery time is longer than perian insect powder, percentage rate of reviving Lower than perian insect powder.According to incompletely statistics, Azalea pontica stinkbug flat to bean, sugar cane cottony aphid, a Boehmeria Huang a kind of butterfly harmful to crop plants, cabbage butterfly, pachydiplosis oryzae, rice 10 section more than the 50 kind Important Economic insect toxic effects such as locust, rice plant skipper, scotellaris, leafhopper, Rhizoma Dioscoreae esculentae leaf beetle, red spider are good, Therefore, Zeng Zuowei soil pesticide is extensively applied in Azalea pontica producing region.
In Rhododendron, number of types of active component is the most studied, such as yellow hair Cuculus polioephalus, Japan Cuculus polioephalus etc..At present from Huang The active component separating and identifying structure in Cuculus polioephalus has 8 kinds: be respectively Chinese azalea extract-II, III, V, Rhodomollein- I, II, III, Kalmanol and Grayanotoxin-III.Additionally, possibly together with Andromedotoxin, Chinese photinia element, rhodotoxin, department's handkerchief Draw husky phenol, aseboquercitrin etc..
Ericad distribution is wide, and wide in variety, its active component kind is many, and activity is high, and purposes is wide, has wide opening The prospect of sending out, China's ericad aboundresources, we should strengthen research and be developed application.
At present, there is not yet employing supercritical CO2The report of Cuculus polioephalus active component is spent in extraction florescence in vain, also there are no relevant Patent.
The present invention with florescence spend in vain Cuculus polioephalus for extract raw material, utilize supercritical CO2Extracting process carries out biological activity one-tenth The extraction divided separates, and it is easy and simple to handle, method is simple, extraction efficiency high.
Summary of the invention
The technical problem to be solved in the present invention is to overcome existing defect, it is provided that a kind of extraction ratio is high, energy consumption is low, operation Easy spends the new process for extracting of bioactive ingredients in Cuculus polioephalus in vain.
In order to solve technique scheme, the invention provides following technical scheme:
The method of bioactive ingredients in Cuculus polioephalus is spent in a kind of extraction in vain, and extraction is put in spending in vain after Cuculus polioephalus is pulverized of being plucked florescence In still, with CO2Fluid is extractant, and extraction temperature is 35-45 DEG C, extracting pressure 15-25MPa, extraction time are 1.5-2.5h, Obtain the extract of flaxen active component.
As preferably, the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried.
The benefit that open air is dried under field conditions (factors) is: purpose is that the moisture allowing and spending Cuculus polioephalus in vain is slow at a temperature of natural environment Slowly evaporate contained humidity, and do not destroy its organizational structure or lose chemical composition contained by other.
As preferably, 200 mesh sieves are crossed in spending in vain after Cuculus polioephalus is pulverized of being plucked florescence.
The purpose selecting this powder particle diameter is: on the one hand be to try to not destroy the organizational structure spending Cuculus polioephalus in vain, on the other hand It is to easily facilitate extraction under the conditions of this granularity.
As preferably, described extracting pressure is 25MPa, extraction temperature is 40 DEG C.
As preferably, response time during described extraction is 2.5h.
The method have the advantages that
Supercritical CO2Extraction is with nontoxic, the supercritical CO of noresidue2Water or organic solvent is replaced to make Extraction solvent, not only Can extract under conditions of room temperature, and high selective extraction and separation can realized, thus obtain high-quality product Product.And supercritical CO2Extraction will not produce the three wastes, extremely advantageous to environmental conservation, extracts material C O2Cheap and easy to get, capable of circulation Using, production cost is relatively low.
In the process parameters range that the present invention provides, spend bioactive ingredients in Folium Rhododendri Simsii in vain for pluck florescence Extraction efficiency is high, and extraction rate is fast, and technique is simple, saves reagent, and power consumption is few, low cost, pollutes few, is better than other and uses tradition The extracting method of extractive technique.
Accompanying drawing explanation
Accompanying drawing is for providing a further understanding of the present invention, and constitutes a part for description, with the reality of the present invention Execute example together for explaining the present invention, be not intended that limitation of the present invention.In the accompanying drawings:
Fig. 1 is for spending Cuculus polioephalus GC/MS chemical composition analysis collection of illustrative plates in vain.
Detailed description of the invention
Below example facilitates a better understanding of the present invention, but does not limit the present invention.Experiment in following embodiment Method, if no special instructions, is conventional method.Test material used in following embodiment, if no special instructions, is city Sell.
1, material and method
1.1 instruments and reagent material
Agilent gaseous mass analyzer (Agilent 6890-5973 GC/MS);Spend Folium Rhododendri Simsii florescence in vain to pluck from autonomy for Tibet District;The chemical reagent such as chloroform are chromatographically pure.
1.2 extracting method
1.2.1 Cuculus polioephalus Feedstock treating is spent florescence in vain
Open air under Folium Rhododendri Simsii natural conditions will be spent florescence in vain dry, after pulverizing, cross 200 mesh sieves, standby.
1.2.2 active component extracts
Precision weighs spends Cuculus polioephalus in vain in extraction kettle, with CO the florescence after 3g-3.8g pulverizes2Fluid is extractant, carries Take, collect the faint yellow extract of 0.00561g-0.02934g from connecing sample mouth, dissolve standby with chloroform.
1.2.3 sample detection condition
Injector temperature: 270 DEG C, heating schedule: 60 DEG C, rise to 280 DEG C with 10 DEG C/min speed, keep 5min, with 5 DEG C/ Min speed rises to 290 DEG C, keeps 3min, split sampling, split ratio: 20:1, carrier gas: high-purity helium, purity >=99.999%, stream Speed 1.0 mL/min.Sample size: 1 μ L.
2. result of the test
The optimum results of 2.1 extraction ratio influence conditions
Select and total extraction ratio has been had (extracting pressure Mpa, extraction temperature DEG C, the extraction time h) consideration of 3 factors of main impact Three levels, with L9(33) orthogonal table carry out test influence factor optimize.Optimum results is shown in Table 1, table 2, table 3.
Table 1 L9(33) orthogonal test influence factor's water-glass
Table 2 L9(33) orthogonal experiments
Table 3L9(33) orthogonal test variance analysis
In scope of experiment, it is considered to extracting production cost, optimum extraction condition is A3B2C1, i.e. spending Cuculus polioephalus pulverizing florescence in vain is 200 mesh, extracting pressure 25MPa, extraction temperature are 40 DEG C, response time 2.5h is optimum extraction condition.
2.2 GC/MS Analysis of test results
(i.e. spending Cuculus polioephalus florescence in vain and pulverizing is 200 mesh, extracting pressure 25MPa, extraction temperature will to apply above-mentioned optimum extraction conditions Be 40 DEG C, response time 2.5h) extract spend in vain Cuculus polioephalus active component use Gas chromatographyMass spectrometry be measured, Referring specifically to Fig. 1,24 kinds of higher compounds of content are isolated in detection altogether;Warp and mass spectrogram data base's comparison, Preliminary Identification Predominantly alkane and containing oxygen derivative (62.32%), alkene and the compound such as alcohol (8.09%), ester (4.87%), wherein include and carry Squalene (content reaches 4.79%) the isoreactivity composition of high immunity of organisms and antitumor action.
Embodiment 1
It is as follows that the method for bioactive ingredients in Cuculus polioephalus is spent in the extraction of the present invention in vain:
(1) the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried, after pulverizing, cross 200 mesh sieves;
(2) weigh 3 g to spend Cuculus polioephalus powder body in vain and put in extraction kettle, with CO2Fluid is extractant, extracting pressure 15MPa, extraction temperature Degree is 35 DEG C, extraction time is 2h, obtains the flaxen active component extract of 0.01034g.
Embodiment 2
It is as follows that the method for bioactive ingredients in Cuculus polioephalus is spent in the extraction of the present invention in vain:
(1) the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried, after pulverizing, cross 200 mesh sieves;
(2) weigh 3.5g to spend Cuculus polioephalus powder body in vain and put in extraction kettle, with CO2Fluid is extractant, extracting pressure 20MPa, extraction Temperature is 45 DEG C, extraction time is 1.5h, obtains the flaxen active component extract of 0.01229g.
Embodiment 3
It is as follows that the method for bioactive ingredients in Cuculus polioephalus is spent in the extraction of the present invention in vain:
(1) the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried, after pulverizing, cross 200 mesh sieves;
(2) weigh 3.7g to spend Cuculus polioephalus powder body in vain and put in extraction kettle, with CO2Fluid is extractant, extracting pressure 25MPa, extraction Temperature is 40 DEG C, extraction time is 2.5h, obtains the flaxen active component extract of 0.02934g.
Embodiment 4
It is as follows that the method for bioactive ingredients in Cuculus polioephalus is spent in the extraction of the present invention in vain:
(1) the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried, after pulverizing, cross 200 mesh sieves;
(2) weigh 3.5g to spend Cuculus polioephalus powder body in vain and put in extraction kettle, with CO2Fluid is extractant, extracting pressure 25MPa, extraction Temperature is 35 DEG C, extraction time is 1.5h, obtains the flaxen active component extract of 0.01876g.
Embodiment 5
It is as follows that the method for bioactive ingredients in Cuculus polioephalus is spent in the extraction of the present invention in vain:
(1) the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried, after pulverizing, cross 200 mesh sieves;
(2) weigh 3.4g to spend Cuculus polioephalus powder body in vain and put in extraction kettle, with CO2Fluid is extractant, extracting pressure 25MPa, extraction Temperature is 45 DEG C, extraction time is 2h, obtains the flaxen active component extract of 0.01808g.
Embodiment 6
It is as follows that the method for bioactive ingredients in Cuculus polioephalus is spent in the extraction of the present invention in vain:
(1) the Cuculus polioephalus open air under field conditions (factors) of spending in vain that florescence plucks is dried, after pulverizing, cross 200 mesh sieves;
(2) weigh 3.8g to spend Cuculus polioephalus powder body in vain and put in extraction kettle, with CO2Fluid is extractant, extracting pressure 15MPa, extraction Temperature is 45 DEG C, extraction time is 2.5h, obtains the flaxen active component extract of 0.00561g.
Finally it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, Although being described in detail the present invention with reference to previous embodiment, for a person skilled in the art, it still may be used So that the technical scheme described in foregoing embodiments to be modified, or wherein portion of techniques feature is carried out equivalent. All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's Within protection domain.

Claims (5)

1. the method for bioactive ingredients in Cuculus polioephalus is spent in an extraction in vain, it is characterised in that: that is plucked florescence spends Cuculus polioephalus in vain Put into after pulverizing in extraction kettle, with CO2Fluid is extractant, and extracting pressure 15-25MPa, extraction temperature are 35-45 DEG C, extraction Time is 1.5-2.5h, obtains the extract of flaxen active component.
Method the most according to claim 1, it is characterised in that: that is plucked florescence spends Cuculus polioephalus family under field conditions (factors) in vain Dry outward.
Method the most according to claim 1, it is characterised in that: 200 mesh are crossed in spending in vain after Cuculus polioephalus is pulverized of being plucked florescence Sieve.
Method the most according to claim 1, it is characterised in that: described extracting pressure is 25MPa, extraction temperature is 40 DEG C.
Method the most according to claim 1, it is characterised in that: response time during described extraction is 2.5h.
CN201610848272.6A 2016-09-26 2016-09-26 The method of bioactive ingredients in Cuculus polioephalus is spent in a kind of extraction in vain Pending CN106265852A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110684599A (en) * 2019-10-24 2020-01-14 江西中烟工业有限责任公司 Preparation method of azalea absolute oil suitable for cigarettes
CN115192624A (en) * 2022-05-23 2022-10-18 成都杨天万应制药有限公司 Extraction process and application of rhododendron Liangshan

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张烨等: ""大白花杜鹃总黄酮提取工艺的优化"", 《南方农业学报》 *
钱伟光等: ""超临界 CO2 萃取烈香杜鹃挥发油的工艺研究"", 《西北药学杂志》 *
陈君等: ""离子液体-超声辅助萃取 /高效液相色谱法测定白花杜鹃叶中的黄酮"", 《分析测试学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110684599A (en) * 2019-10-24 2020-01-14 江西中烟工业有限责任公司 Preparation method of azalea absolute oil suitable for cigarettes
CN115192624A (en) * 2022-05-23 2022-10-18 成都杨天万应制药有限公司 Extraction process and application of rhododendron Liangshan
CN115192624B (en) * 2022-05-23 2023-10-13 成都杨天万应制药有限公司 Extraction process and application of rhododendron simsii

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