CN101288694A - Preparation method of magnolia bark extracts with no residual solvent, low oiliness and high content - Google Patents

Preparation method of magnolia bark extracts with no residual solvent, low oiliness and high content Download PDF

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Publication number
CN101288694A
CN101288694A CNA2007100777231A CN200710077723A CN101288694A CN 101288694 A CN101288694 A CN 101288694A CN A2007100777231 A CNA2007100777231 A CN A2007100777231A CN 200710077723 A CN200710077723 A CN 200710077723A CN 101288694 A CN101288694 A CN 101288694A
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China
Prior art keywords
temperature
cortex magnoliae
magnoliae officinalis
pressure
oiliness
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CNA2007100777231A
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Chinese (zh)
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田弋夫
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Institute of Geochemistry of CAS
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Institute of Geochemistry of CAS
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Priority to CNA2007100777231A priority Critical patent/CN101288694A/en
Publication of CN101288694A publication Critical patent/CN101288694A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a preparation method for magnolia officinalis extract with no residue, low oiliness and high content. The invention is characterized in that tree bark, root bark and branch bark are taken as raw materials, supercritical CO2 fluid extraction and multi-stage separation technology is adopted to get magnolia officinalis extract, and the content of magnolol and honokiol is more than 90 percent. The magnolia officinalis extract has the advantages of no organic solvent residue, low oiliness, easy crushability and good dispersibility, which can be used directly in the production of dosage forms such as tablets and capsules, etc.

Description

A kind of preparation method of not having molten residual, low oiliness, high-load Cortex Magnoliae Officinalis extract
Technical field
The present invention relates to a kind of effective ingredients in plant preparation method of extract.
Background technology
Cortex Magnoliae Officinalis is dried bark, root bark or the branch skin of Magnoliacea plant Cortex Magnoliae Officinalis (Magnolia officinalis Rehd.et Wils.) or magnolia officinalis rehd.et wils.var.biloba rehd.et wils. (Magnolia officinalis Rehd.et Wils.Var.biloba Rehd.et Wils), tcm clinical practice has dampness expectorant, the therapeutic method to keep the adverse QI flowing downwards except that full effect as damp-resolving medicinal.Modern pharmacology studies show that, Cortex Magnoliae Officinalis has the activity of the gastrointestinal of influence, antibiotic, antiviral, of flaccid muscles and effects such as maincenter inhibition, antiallergic.Main effective ingredient in the Cortex Magnoliae Officinalis is magnolol and honokiol.Modern study shows that magnolol and honokiol have stronger antifungal, anti-inflammatory effect, simultaneously nervous system, cardio-cerebrovascular is had good action, finds also that in recent years it has antitumor and anti-aging effects.
Generally use in the commercial production such as pharmacy in the Cortex Magnoliae Officinalis extract mode.General Cortex Magnoliae Officinalis extract production is to adopt organic solvent extraction, and the active constituent content of product is low, needs further refining; Production efficiency is low, the solvent recovery loss is big; Containing certain dissolvent residual in the product is unfavorable for using in specialities (as medicine, daily chemical products).Also the someone uses supercritical technology production, but because separating technology is undesirable, makes and contain more oily matter in the product, the product oiliness weighs, easily lumps agglomerating, bad dispersibility can not be directly used in the production of tablet, capsule etc., also needs to remove oily matter through certain solvent processing.
Summary of the invention
The objective of the invention is to propose to adopt no molten residual, the method for hanging down oiliness, Cortex Magnoliae Officinalis extract that effective ingredient is high of supercritical fluid extraction and the preparation of multiple stage separation technology.
The specific embodiment
The present invention implements as follows: bark, root bark, branch skin with Cortex Magnoliae Officinalis are that raw material is through being crushed to suitable granularity, the input supercritical CO 2In the fluid extraction device at extracting pressure 15~40Mpa, 30~60 ℃ of extraction temperature; Flash trapping stage pressure 10~15Mpa, 40~60 ℃ of temperature; Secondary separating pressure 8~10Mpa, 40~60 ℃ of temperature; Three grades of disjoining pressure power 5~8Mpa, 40~60 ℃ of temperature, CO 2Carry out under the suitable condition of flow.
The Cortex Magnoliae Officinalis root bark of example 1 after the supercritical CO of packing into 0.5 kilogram of pulverizing 2In the extraction kettle of fluid extraction device, it is pressure 25Mpa that extraction conditions is set, 50 ℃ of extraction temperature; Flash trapping stage pressure 11Mpa, 55 ℃ of temperature; Secondary separating pressure 9Mpa, 55 ℃ of temperature; Three grades of disjoining pressure power 7Mpa, 55 ℃ of temperature, suitable CO2 flow carries out extract and separate.Obtain 0.05 kilogram of white or off-white powder shape Cortex Magnoliae Officinalis extract from the flash trapping stage still, wherein magnolol and honokiol content are 94.6%, oiliness material hardly, and good dispersion can be pulverized 60 mesh sieves; It is dynamic to obtain being semi-fluid under 0.02 kilogram of high temperature of yellow block from the secondary separating still, and magnolol and honokiol content are 65.7%, and oiliness is heavier, pulverizes easily caking of back; It is dynamic to obtain being semi-fluid under 0.01 kilogram of room temperature of yellow block from three grades from still, and magnolol and honokiol content are 37.8%, and oiliness is very heavy, is difficult for pulverizing.
The Cortex Magnoliae Officinalis root bark of example 2 after the supercritical CO of packing into 5 kilograms of pulverizing 2In the extraction kettle of fluid extraction device, it is pressure 25Mpa that extraction conditions is set, 50 ℃ of extraction temperature; Flash trapping stage pressure 11Mpa, 55 ℃ of temperature; Secondary separating pressure 9Mpa, 55 ℃ of temperature; Three grades of disjoining pressure power 7Mpa, 55 ℃ of temperature, suitable CO2 flow carries out extract and separate.Obtain 0.48 kilogram of white or off-white powder shape Cortex Magnoliae Officinalis extract from the flash trapping stage still, wherein magnolol and honokiol content are 93.7%, oiliness material hardly, and good dispersion can be pulverized 60 mesh sieves; It is dynamic to obtain being semi-fluid under 0.25 kilogram of high temperature of yellow block from the secondary separating still, and magnolol and honokiol content are 63.8%, and oiliness is heavier, pulverizes easily caking of back; It is dynamic to obtain being semi-fluid under 0.13 kilogram of room temperature of yellow block from three grades from still, and magnolol and honokiol content are 34.8%, and oiliness is very heavy, is difficult for pulverizing.
The Cortex Magnoliae Officinalis root bark of example 3 after the supercritical CO of packing into 25 kilograms of pulverizing 2In the extraction kettle of fluid extraction device, it is pressure 25Mpa that extraction conditions is set, 50 ℃ of extraction temperature; Flash trapping stage pressure 11Mpa, 55 ℃ of temperature; Secondary separating pressure 9Mpa, 55 ℃ of temperature; Three grades of disjoining pressure power 7Mpa, 55 ℃ of temperature, suitable CO2 flow carries out extract and separate.Obtain 2.6 kilograms of white or off-white powder shape Cortex Magnoliae Officinalis extracts from the flash trapping stage still, wherein magnolol and honokiol content are 92.3%, oiliness material hardly, and good dispersion can be pulverized 60 mesh sieves; It is dynamic to obtain being semi-fluid under 1.2 kilograms of high temperature of yellow block from the secondary separating still, and magnolol and honokiol content are 60.8%, and oiliness is heavier, pulverizes easily caking of back; It is dynamic to obtain being semi-fluid under 0.9 kilogram of room temperature of yellow block from three grades from still, and magnolol and honokiol content are 30.8%, and oiliness is very heavy, is difficult for pulverizing.

Claims (3)

1. the preparation method of no molten residual, a low oiliness, high-load Cortex Magnoliae Officinalis extract.Feature is that bark, root bark, the branch skin with Cortex Magnoliae Officinalis is raw material, adopt supercritical C02 fluid extraction and multiple stage separation technology, obtain Cortex Magnoliae Officinalis extract, its magnolol and honokiol content are greater than 90%, organic solvent-free is residual, oiliness is low, easily pulverizing, good dispersion can be directly used in the production of dosage forms such as tablet, capsule.It is characterized in that bark, root bark, branch skin with Cortex Magnoliae Officinalis are raw material, carry out the supercritical CO 2 extraction under the condition, under condition, carry out then; Under condition, carry out; Under condition, carry out three grades of separation; Obtain Cortex Magnoliae Officinalis extract, magnolol and honokiol content are greater than 90%, and organic solvent-free is residual, oiliness is low, and easily pulverizing, good dispersion can be directly used in the production of dosage forms such as tablet, capsule.
2. Cortex Magnoliae Officinalis extract production method according to claim 1, production main technologic parameters are extracting pressure 15~40Mpa, 30~60 ℃ of extraction temperature; Flash trapping stage pressure 10~15Mpa, 40~60 ℃ of temperature; Secondary separating pressure 8~10Mpa, 40~60 ℃ of temperature; Three grades of disjoining pressure power 5~8Mpa, 40~60 ℃ of temperature.
3. Cortex Magnoliae Officinalis extract production method according to claim 1, best manufacturing technology are extracting pressure 25Mpa, 50 ℃ of extraction temperature; Flash trapping stage pressure 11Mpa, 55 ℃ of temperature; Secondary separating pressure 9Mpa, 55 ℃ of temperature; Three grades of disjoining pressure power 7Mpa, 55 ℃ of temperature.
CNA2007100777231A 2007-04-16 2007-04-16 Preparation method of magnolia bark extracts with no residual solvent, low oiliness and high content Pending CN101288694A (en)

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Application Number Priority Date Filing Date Title
CNA2007100777231A CN101288694A (en) 2007-04-16 2007-04-16 Preparation method of magnolia bark extracts with no residual solvent, low oiliness and high content

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CN101288694A true CN101288694A (en) 2008-10-22

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101735021A (en) * 2008-11-26 2010-06-16 湖南农业大学 Method for separating and purifying magnolol and honokiol by HP-20 macroporous resin
CN102041163A (en) * 2011-01-05 2011-05-04 南昌同心紫巢生物工程有限公司 Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil
CN113730440A (en) * 2021-09-14 2021-12-03 康博士日化集团有限公司 Antibacterial composition and oral care product containing same

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101735021A (en) * 2008-11-26 2010-06-16 湖南农业大学 Method for separating and purifying magnolol and honokiol by HP-20 macroporous resin
CN101735021B (en) * 2008-11-26 2013-03-06 湖南农业大学 Method for separating and purifying magnolol and honokiol by HP-20 macroporous resin
CN102041163A (en) * 2011-01-05 2011-05-04 南昌同心紫巢生物工程有限公司 Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil
CN102041163B (en) * 2011-01-05 2013-04-17 南昌同心紫巢生物工程有限公司 Multi-body multi-stage supercritical CO2 method for extraction of ganoderma lucidum spore oil
CN113730440A (en) * 2021-09-14 2021-12-03 康博士日化集团有限公司 Antibacterial composition and oral care product containing same

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Open date: 20081022