CN1234671C - Molecular distillation purification method of polyprenol - Google Patents
Molecular distillation purification method of polyprenol Download PDFInfo
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- CN1234671C CN1234671C CN 200410041670 CN200410041670A CN1234671C CN 1234671 C CN1234671 C CN 1234671C CN 200410041670 CN200410041670 CN 200410041670 CN 200410041670 A CN200410041670 A CN 200410041670A CN 1234671 C CN1234671 C CN 1234671C
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Abstract
The present invention relates to a molecular distillation purification method of polyprenol, which comprises: step one, feeding paste containing below 50% of polyprenol at the flow speed of 3 to 15 ml/min into a molecular distilling evaporator with a vacuum degree of 1*10<-2>mbar to 10* 10<-2>mbar and at the temperature of 80 to 160 DEG C for distillation to obtain I grade molecular distillation residue; step two, feeding the I grade molecular distillation residue at the flow speed of 5 to 15 ml/min into another molecular distilling evaporator with a vacuum degree of 1*10<-3>mbar to 5* 10<-3>mbar and at the temperature of 160 to 300 DEG C for distillation to obtain II grade molecular distillation residue containing 70% to 95% of polyprenol. Molecular distillation products obtained by the present invention have no solvent residue to overcome the problems of large loss and high cost for recovering various mixed solvents.
Description
Technical field
The present invention relates to a kind of plant polyprenol and extract and isolation technique, relate in particular to a kind of molecular distillation purification process of polyprenol.
Background technology
Polyprenol extensively is present in the higher plant, we studies show that, polyprenol mainly is present in the green needles such as Ginkgo Leaf and Pinus massoniana Lamb, black pine, slash pine, Chinese juniper, cdear in China, but secondly the content in Ginkgo Leaf contain about 1.0% in needles such as Pinus massoniana Lamb, cdear, black pine up to 2.0%.The lipoid cpd that polyprenol (Polyprenols) is made up of a series of isopentene groups unit and terminal prenol unit.They all have the chemical structure of birch polyprenol (Butalpolyprenols), be that (wherein n is 10-21 to 2-(cis) the n-α of ω-(trans), α is a prenol), (the Dolichols structure is 2-(cis) the n-α of ω-(trans) to contained dolichol (Dolichols) structure in they and human body and the Mammals internal organs, wherein n is 12-19, α is a primary isoamyl alcohol) approaching, and can in human body, be metabolized to dolichol.
Latvia mainly utilizes needles such as Scots pine, dragon spruce to separate the polyprenol (m=2-3, n=8-16) of preparation alltrans polyprenol (m=9) and 10-18 isopentene group unit number with Russia; The Latvia woods is ground the silicagel column isolation technique that adopts and has set up the production equipment of producing one kilogram of polyprenol daily, but does not see the patent report.The chemical ingredients and the separation method of there has been patent report in Japan Ginkgo Leaf and cdear needle polyprenol, but the multiple solvent extraction of this method, silicagel column separates earlier preparation polyprenol acetic ester, is hydrolyzed into polyprenol again, carry out methods such as solvent is freezing, silicagel column separation then, technology is loaded down with trivial details, the product yield only has 0.2%-0.3%, and the cost height can't suitability for industrialized production.
The domestic king publication (CN1392167A, 2001) of coming out as an article has been reported Ginkgo Leaf polyprenol and Folium Ginkgo extract preparation (GBE) method, is characterized in producing simultaneously polyprenol and GBE.Multiple solvent extraction of its process using and solvent frozen preparation 50% above Ginkgo Leaf polyprenol ointment, through silicagel column or polymeric adsorbent Processing of Preparation 70% above polyprenol oily matter, the product yield is about 0.5% again.Though this method is industrialized mass production, the separation of multiple solvent and cost recovery height, loss is bigger, and dissolvent residual is still a problem in the product.Yang Xiaoming has proposed a kind of breadboard method, promptly adopts silica gel thin-layer and silica gel column chromatography to prepare the polyprenol homologue, and its cost is very high, can't realize batch preparations in practice.The Yankee enlightening is with the method (Ginkgo Leaf polyprenol compounds separating technology grinds Guangxi University's journal) of NKA macroporous resin and silica gel column chromatography, and polyprenol content is refined to 70% less than 50% Ginkgo Leaf ointment.But with non-polar solvent (sherwood oil, ether, ethyl acetate etc.), and nonpolar dissolubility is the auxiliary agent stripping in the NKA resin voids when desorbing the NKA resin, and the residual quantity of auxiliary agent is very big in the product, and is difficult for steaming.
Therefore, tradition is separated the method for preparing polyprenol and had three significant disadvantages: 1. when silica gel separated preparation with aluminum oxide, silica gel and aluminum oxide regeneration were problems, the cost height.2. adopt different ratios mixed extractant solvents such as sherwood oil, ether, acetone, ethyl acetate when conciliating the attached column chromatography, not only solvent load is big, and it is big to reclaim when separating solvent loss, the cost height.3. the residue problem that has solvent in Zhi Bei the polyprenol product.
Summary of the invention
The present invention proposes a kind of low cost, need not the molecular distillation purification process of the polyprenol of organic solvent.
The present invention adopts following technical scheme:
A kind of molecular distillation purification process of polyprenol is characterized in that comprising following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment and sends into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in 80 ℃～160 ℃ the molecular distillation vaporizer and distill, and can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum.
Inventive principle: the present invention proposes to adopt molecular distillation technique purifying polyprenol, is according to chemical ingredients difference in the Ginkgo Leaf non-polar solvent extract ointment, the principle that its molecular weight difference is big.Studies show that: Ginkgo Leaf non-polar solvent extract ointment is fat-soluble component, is made up of essential oil, acid and neutrals.Acid is a free acid, is mainly higher fatty acid and a spot of organic phenolic acid.Higher fatty acid accounts for 62.3%, and wherein saturated fatty acid accounts for 45.6%, is made up of C12, C14, C16, C18 and C20, mainly is C16 saturated acid (34.4%); Unsaturated fatty acids accounts for 53.9%, is made up of C18:1, C18:2, C18:3 and C18:4, mainly is C18:1 (15%) and C18:3 (32.8%).Neutrals accounts for 76.8% in Ginkgo Leaf Petroleum ether extraction ointment, can be divided into combined acid and unsaponifiables through saponification.Unsaponifiables mainly by pigment (comprising carotene, xenthophylls), wax, high fatty alcohol, polypenthylene alcohols, terpene alcohols, sterols, contain oxygen multi-functional compounds (as aldehydes, ketone) etc. and form.Detect through TLC, wherein the Rf value of polypenthylene alcohols is about 0.52.And the Rf value littler may be that compounds such as the bigger Fatty Alcohol(C12-C14 and C12-C18) of polarity, phytol and other contain oxygen more function group compound (as aldehydes, ketone).Classes of compounds polarity difference in the Ginkgo Leaf ointment, especially molecular weight difference, wherein essential oil, wax, acid, ester class, Fatty Alcohol(C12-C14 and C12-C18), sterol equimolecular quantity are relatively little, boiling point is relatively low, and polyprenol, pigment, to contain oxygen multi-functional compounds molecular weight big relatively, boiling point is high relatively, especially polyprenol compounds molecular-weight average is greater than 1000, therefore can utilize molecular distillation and molecule short-path distillation technology under very low vacuum, they to be separated, reach the purpose of purifying polyprenol.Prepare in the 70%-95% polyprenol oily matter technology in the present invention, polyprenol content being lower than 50% ointment sends in the vaporizer of molecular distillation, select vacuum tightness and vaporization temperature, regulate ointment charging flow velocity, scraper plate rotating speed, polyprenol ointment is carried out the stepwise distillation processing.I level molecule fractionation by distillation light oil-1 part (comprising essential oil, wax, acid, Fatty Alcohol(C12-C14 and C12-C18) and a small amount of organic solvent), the isolated part of II molecular distillation is light oil-2 (glycerine trigalloyl ester, sterol, an xenthophylls etc.), be faint yellow fat-soluble oily matter, the residue of II molecular distillation is brown heavy oil part, i.e. polyphosphazene polymer pentenol enrichment section (polypenthylene alcohols, pigment, contain oxygen multi-functional compounds etc.).As shown in table 1.
Table 1. molecular distillation extracts the separation of chemical ingredients in the ointment to Ginkgo Leaf
| The molecular distillation processing condition | Rectifying section | Appearance property | Main component |
| 1-10×10 -2mbar. 80-160℃ | Light oil-1 part | Faint yellow oily thing, viscosity is low | Essential oil, wax, acid, Fatty Alcohol(C12-C14 and C12-C18) and a small amount of solvent etc. |
| 1-5×10 -3mbar. 180-300℃ | Light oil-2 part | Yellow oil, viscosity is low | Glycerine trigalloyl ester, sterol, xenthophylls etc. |
| 1-5×10 -3mbar. 180-300℃ | The heavy oil part | Dark-brown oily matter is thicker | Polyphosphazene polymer pentenol enrichment section (polypenthylene alcohols, pigment, contain oxygen multi-functional compounds etc.) |
The present invention obtains following technique effect:
(1) with respect to prior art, the present invention utilizes the less easy evaporation of the molecular weight of impurity in the raw material, and the molecular weight of polyprenol big (average out to 1000), not evaporable principle and polyprenol content is lower than the distillation of 50% ointment purifies and be the polyprenol oily matter of 70%-95%, in the distillation of I level molecule, boil off small molecules, in the distillation of II level, boil off medium sized molecule, improved the purity of polyprenol in the product, and do not need organic solvent, therefore there is not dissolvent residual in the product of molecular distillation, overcome the problem that loss was big and cost is high when multiple mixed solvent reclaimed, thereby greatly reduced production cost.
(2) the present invention only adopts molecular distillation isolation technique purifying polyprenol content to be lower than 50% ointment, the polyprenol oily matter of refining 70%-95%, not only overcome the shortcoming of traditional refining polyprenol method, and the quality of product is more stable, its chemical constitution remains unchanged.
(3) the present invention carries out the knifing processing to material respectively in distillation of I level molecule and the distillation of II level molecule, has increased molecular distillation speed.
(4) the present invention adopts Ginkgo Leaf and coniferous species to prepare polyprenol content to be lower than 50% ointment, because Ginkgo Leaf and coniferous species are more common seeds, output is big, wide material sources and abundance, thereby when comprehensive process Ginkgo Leaf and coniferous species, can reduce the production cost that polyprenol content is lower than 50% ointment greatly, the residual leaf after Folium Ginkgo extract (GBE) is produced also is rich in polyprenol, thereby utilization of waste material further can be reduced cost.
Ginkgo Leaf provided by the present invention or needle non-polar solvent extract ointment, be with sherwood oil, normal hexane, the lixiviate of industrial naptha equal solvent, concentrate, the ointment of preparations such as hydrolysis, extraction or resin absorption, be the polyprenol raw product, wherein the content of polyprenol is lower than 50%.
In the present invention, the polyprenol analysis on Content is quantitative with high performance liquid chromatography, chromatographic column is Kromasil ODS1C18 (I.D.4.6mm * 250mm, 5 μ m), ultraviolet detection, the detection wavelength is 210nm, moving phase is Virahol: methyl alcohol=1: 1 (v/v), flow velocity are 1.0ml/min., are standard substance with the C60 polyprenol, the peak area external standard method is quantitative, the total content of polyprenol in the working sample.
Embodiment
The molecular distillation purification process of 1 one kinds of polyprenols of embodiment, comprise following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment (production of scientific and technological development main office of Chinese forest-science academy woodsization institute) sends into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in distillation in 80 ℃～160 ℃ the molecular distillation vaporizer (KDL5 type, German U.I.C.GMBH company produces), and in the present embodiment, flow velocity can be 5ml/min, 8ml/min, and 10ml/min, 13.2ml/min, vacuum tightness can be 3 * 10
-2Mbar, 5 * 10
-2Mbar, 8 * 10
-2Mbar, temperature can be 92 ℃, 105 ℃, 109 ℃, 117 ℃, 130 ℃, 142 ℃, 155 ℃, topping-1 can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, and in the present embodiment, flow velocity can be 1.7 * 10
-3Mbar, 2.5 * 10
-3Mbar, 3.2 * 10
-3Mbar, 3.8 * 10
-3Mbar, 4.1 * 10
-3Mbar, 4.7 * 10
-3Mbar, temperature can be 175 ℃, 188 ℃, 220 ℃, 235 ℃, 255 ℃, 276 ℃, 290 ℃, topping-2, can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum.
The molecular distillation purification process of 2 one kinds of polyprenols of embodiment, comprise following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment China forest-science academy scientific and technological development main office of woodsization institute production) send into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in distillation in 80 ℃～160 ℃ the molecular distillation vaporizer (KDL5 type, German U.I.C.GMBH company produces), and in the present embodiment, flow velocity can be 5ml/min, 8ml/min, and 10ml/min, 13.2ml/min, vacuum tightness can be 3 * 10
-2Mbar, 5 * 10
-2Mbar, 8 * 10
-2Mbar, temperature can be 92 ℃, 105 ℃, 109 ℃, 117 ℃, 130 ℃, 142 ℃, 155 ℃, topping-1 can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, and in the present embodiment, flow velocity can be 1.7 * 10
-3Mbar, 2.5 * 10
-3Mbar, 3.2 * 10
-3Mbar, 3.8 * 10
-3Mbar, 4.1 * 10
-3Mbar, 4.7 * 10
-3Mbar, temperature can be 175 ℃, 188 ℃, 220 ℃, 235 ℃, 255 ℃, 276 ℃, 290 ℃, topping-2, can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum, in the present embodiment, can be that 250rpm～300rpm carries out knifing with the knifing rotating speed to the material in the I level molecule distillation evaporative process in the molecular distillation vaporizer, can be that 300rpm～450rpm carries out knifing with the knifing rotating speed to the material in the II level molecule distillation evaporative process.
The molecular distillation purification process of 3 one kinds of polyprenols of embodiment comprises following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment and sends into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in distillation in 80 ℃～160 ℃ the molecular distillation vaporizer (KDL5 type, German U.I.C.GMBH company produces), and in the present embodiment, flow velocity can be 5ml/min, 8ml/min, and 10ml/min, 13.2ml/min, vacuum tightness can be 3 * 10
-2Mbar, 5 * 10
-2Mbar, 8 * 10
-2Mbar, temperature can be 92 ℃, 105 ℃, 109 ℃, 117 ℃, 130 ℃, 142 ℃, 155 ℃, topping-1 can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, and in the present embodiment, flow velocity can be 1.7 * 10
-3Mbar, 2.5 * 10
-3Mbar, 3.2 * 10
-3Mbar, 3.8 * 10
-3Mbar, 4.1 * 10
-3Mbar, 4.7 * 10
-3Mbar, temperature can be 175 ℃, 188 ℃, 220 ℃, 235 ℃, 255 ℃, 276 ℃, 290 ℃, topping-2, can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum, in the present embodiment, polyprenol content is lower than 50% ointment and can obtains by the following method: get the Ginkgo Leaf 5kg that drying contains polyprenol, add 60kg sherwood oil (60 ℃-90 ℃), thermal backflow is extracted, 4 hours time, extract for the second time and add 30kg sherwood oil (60 ℃-90 ℃), operation more than repeating.United extraction liquid, 50 ℃ of most solvents of following reclaim under reduced pressure get sherwood oil (60 ℃-90 ℃) extract 220g, add 3L25% NaOH-EtOH solution, 70 ℃ were reacted 3 hours down, reclaimed ethanol to the greatest extent, add water to 3L, the mixing solutions 2L extraction with sherwood oil and ether repeats 4 times, combining extraction liquid reclaims solvent, gets enriched material 75g: use the 0.5L acetone solution more respectively, filter and remove insolubles, reclaim solvent, get enriched material 48g, be Ginkgo Leaf polyprenol ointment, wherein polyprenol content is 48.6%.
The molecular distillation purification process of 4 one kinds of polyprenols of embodiment comprises following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment and sends into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in distillation in 80 ℃～160 ℃ the molecular distillation vaporizer (KDL5 type, German U.I.C.GMBH company produces), and in the present embodiment, flow velocity can be 5ml/min, 8ml/min, and 10ml/min, 13.2ml/min, vacuum tightness can be 3 * 10
-2Mbar, 5 * 10
-2Mbar, 8 * 10
-2Mbar, temperature can be 92 ℃, 105 ℃, 109 ℃, 117 ℃, 130 ℃, 142 ℃, 155 ℃, topping-1 can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, and in the present embodiment, flow velocity can be 1.7 * 10
-3Mbar, 2.5 * 10
-3Mbar, 3.2 * 10
-3Mbar, 3.8 * 10
-3Mbar, 4.1 * 10
-3Mbar, 4.7 * 10
-3Mbar, temperature can be 175 ℃, 188 ℃, 220 ℃, 235 ℃, 255 ℃, 276 ℃, 290 ℃, topping-2, can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum, in the present embodiment, polyprenol content is lower than 50% ointment and can obtains by the following method: get the residual leaf after Folium Ginkgo extract is produced, put into inherent 80 ℃ of-90 ℃ of dryings of baking oven, the content of moisture content is lower than 5% in the dry leave, is broken into fine powder again.Take by weighing the 400g fine powder, put into return channel, add sherwood oil (60 ℃-90 ℃) 3.2L again, 45 ℃ of-55 ℃ of following lixiviates 4 hours, extraction for the second time added 2.4L sherwood oil (60 ℃-90 ℃), united extraction liquid, 50 ℃ of most solvents of following reclaim under reduced pressure get sherwood oil (60 ℃-90 ℃) extract 21.7g.In the 10%EtOH-of the 0.3L aqueous solution, add 0.3g NaOH, 85 ℃ were reacted 3.5 hours down, reclaim ethanol to the greatest extent, add water to 0.25L, use the 0.4L petroleum ether extraction, repeat 4 times, combining extraction liquid reclaims solvent, gets enriched material 7.05g, be Ginkgo Leaf polyprenol ointment, wherein polyprenol content is 34.5%.
The molecular distillation purification process of 5 one kinds of polyprenols of embodiment comprises following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment and sends into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in distillation in 80 ℃～160 ℃ the molecular distillation vaporizer (KDL5 type, German U.I.C.GMBH company produces), and in the present embodiment, flow velocity can be 5ml/min, 8ml/min, and 10ml/min, 13.2ml/min, vacuum tightness can be 3 * 10
-2Mbar, 5 * 10
-2Mbar, 8 * 10
-2Mbar, temperature can be 92 ℃, 105 ℃, 109 ℃, 117 ℃, 130 ℃, 142 ℃, 155 ℃, topping-1 can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, and in the present embodiment, flow velocity can be 1.7 * 10
-3Mbar, 2.5 * 10
-3Mbar, 3.2 * 10
-3Mbar, 3.8 * 10
-3Mbar, 4.1 * 10
-3Mbar, 4.7 * 10
-3Mbar, temperature can be 175 ℃, 188 ℃, 220 ℃, 235 ℃, 255 ℃, 276 ℃, 290 ℃, topping-2, can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum, in the present embodiment, polyprenol content is lower than 50% ointment and can obtains by the following method: get the fresh needle that contains polyprenol, the needle that contains polyprenol can be Pinus massoniana Lamb or black pine, slash pine, the mixture of one or more in Chinese juniper and the cdear needle is washed to the greatest extent, mixture can be any proportioning, and 60 ℃ of oven dry are ground into powder with pulverizer in baking oven.Get 1kg exsiccant Folium Pini powder, put into the Soxhlet return channel, add the sherwood oil (60 ℃-90 ℃) of 8L, refluxed 10 hours at 60 ℃ of following constant temperature, concentrated extracting solution is at the most solvent of 50 ℃ of following reclaim under reduced pressure, get sherwood oil (60 ℃-90 ℃) extract 22.3g, add 0.3L35%NaOH-H
2O solution, 70 ℃ of down reactions 4 hours, after the cooling, the miscible fluid 0.3L extraction with sherwood oil and ether repeats 3 times, and combining extraction liquid reclaims solvent, gets enriched material 8.6g; Be needle polyprenol ointment, wherein polyprenol content is 24.3%.
Claims (6)
1. the molecular distillation purification process of a polyprenol is characterized in that comprising following two steps: the first step, I level molecule distillation: polyprenol content is lower than 50% ointment and sends into vacuum tightness with the flow velocity of 3ml/min～15ml/min and remain 1 * 10
-2Mbar～10 * 10
-2Mbar, temperature are in 80 ℃～160 ℃ the molecular distillation vaporizer and distill, and can obtain I level molecule distillation residuum, second step, II level molecule distillation: I level molecule distillation residuum is sent into vacuum tightness with flow velocity 5ml/min～15ml/min remain 1 * 10
-3Mbar～5 * 10
-3Mbar, temperature are in 160 ℃～300 ℃ the molecular distillation vaporizer and distill, and can obtain containing the polyprenol mass percent and be 70%～95% II level molecule distillation residuum.
2. the molecular distillation purification process of polyprenol according to claim 1 is characterized in that in I level molecule still-process material being carried out knifing, and the knifing rotating speed is 250rpm～300rpm.
3. the molecular distillation purification process of polyprenol according to claim 1 is characterized in that in II level molecule still-process material being carried out knifing, and the knifing rotating speed is 300rpm～450rpm.
4. the molecular distillation purification process of polyprenol according to claim 1, it is characterized in that polyprenol content is lower than 50% ointment and can obtains by the following method: with containing the Ginkgo Leaf of polyprenol compounds or containing the coniferous species of polyprenol compounds, through art breading such as sherwood oil, normal hexane, the lixiviate of industrial naptha non-polar solvent, hydrolysis, extraction, resin absorption, obtain polyprenol content and be lower than 50% ointment.
5. the molecular distillation purification process of polyprenol according to claim 4 is characterized in that Ginkgo Leaf can be the residual leaf after Folium Ginkgo extract is produced.
6. the molecular distillation purification process of polyprenol according to claim 4 is characterized in that coniferous species is one or more the mixture in Pinus massoniana Lamb, black pine, slash pine, Chinese juniper, the cdear, and the composition of mixture can be any proportioning.
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| CN101381274B (en) * | 2008-10-16 | 2012-05-30 | 中国农业大学 | Method for removing dissolvent residual from lycopene oleoresin |
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| CN102807471A (en) * | 2011-05-30 | 2012-12-05 | 浙江科技学院 | Method for separation preparation of high purity natural phytol |
| CN106810619B (en) * | 2015-12-02 | 2019-01-15 | 中国科学院大连化学物理研究所 | A kind of gingko episperm pectin and polypentenol extracting method |
| CN106262653B (en) * | 2016-08-11 | 2019-08-02 | 广州市名花香料有限公司 | Sulfur-bearing flavor ester composition and preparation method thereof and cheese's essence |
| CN114574284B (en) * | 2020-11-30 | 2024-04-19 | 上海自然堂集团有限公司 | Cedar essential oil, compound Cedar essential oil, extraction method and application thereof |
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| CN101381274B (en) * | 2008-10-16 | 2012-05-30 | 中国农业大学 | Method for removing dissolvent residual from lycopene oleoresin |
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