CN1304081C - Method by extracting samara essence by supercritical CO2 - Google Patents

Abstract

The present invention relates to a method for extracting samara extract by supercritical CO2, which comprises the following steps that full samara fruits rich in phytosterol and other unsaponifiable matter are used as raw materials and pulverized into 10-meshed to 40-meshed powder, and supercritical extraction is carried out on the powder at extraction pressure of 15 to 35MPa at an extraction temperature of 31.1 to 60 DEG C; mixed samara extract with phytosterol is obtained through separation at pressure of 4 to 10MPa at a temperature of 10 to 80 DEG C; and the mixture is made to stand and is precipitated at a temperature of 10 to 25DEGC, solid-liquid separation is carried out by a centrifugation or filtration method, the liquid is samara oil, and the solid is the samara extract. The method has the advantages that the full samara fruits with epicarp are used as raw materials, the samara extract and samara oil products rich in phytosterol vitamin E or the like are obtained and can be extensively applicable to medical care, food, cosmetics and other industries.

Description

Supercritical CO 2Extract the method for samara essence

Technical field

The present invention relates to a kind of from plant material the method for effective component extracting samara essence, be meant the separation and refining method that from the samara fruit, extracts samara essence especially.

Technical background

The plant main body of oil is the glyceride of higher fatty acids.Also contain some unsaponifiable matter in the grease, their content majorities in vegetable oil are about 1%.Though their content is not high, form very abundantly, contain many active materials and comprise phytosterol, vitamins etc., living organism there is very important and special regulatory function.

In the unsaponifiable matter of vegetable oil, phytosterol and phytosterol derivative are subjected to people's welcome, the commercialization of many products deeply because its distinctive biology and physicochemical property are widely used in the industries such as food, medicine, cosmetics.Phytosterol is one of focus of Recent study, the kind of phytosterol is a lot, mainly contains sitosterol, stigmasterol, spinasterol, campesterol and ergosterol etc., and sitosterol has α, β, γ and δ etc. multiple, Yan Jiu maximum cupreol wherein, the molecular formula of cupreol is C ₂₉H ₅₀O.In the technical study of phytosterol separation and Extraction, modal 4 kinds of sterols just, its structural formula is seen Fig. 1. when main ring and side chain respectively have a two key: R=CH ₃The time be brassicasterol, R=C ₂H ₅The time be stigmasterol; During the unparalleled key of side chain perhydrogenate: R=CH ₃, the time be campesterol, R=C ₂H ₅The time be cupreol.

The molecular structure of Fig. 1, common sterol

At drug world, phytosterol can be used for treating tumor of prostate and regulates high cholesterol.Also can be used as the anti-inflammatory conditioning agent.They can be material composition as the synthetic initial substance of steroids for method by microbial fermentation.Estimate that phytosterol substitute demand in the manufacturing of steroids medicine will reach 5000 tons.Phytosterol derivative (as the phytosterol polysaccharide) Chang Zuowei medicine carrier in spraying.In cosmetic industry, phytosterol is commonly used for Skin Cell promoter, antiinflammatory, Wound-healing agent and nonionic emulsifier; Also often with the form (ethoxy compound, polysaccharide, sulfate) of derivative as emulsifying agent and conditioning agent.In food industry, they often appear at as the natural nutrition factor in the prescription of food enrichment and margarine with the treatment high cholesterol, estimate that this aspect use amount can reach 7000 tons.At the herbaceous plant drug world, it can be used as food enrichment.The solid demand of industry demonstrates phytosterol and has fine development prospect.

Elaeagnus mollis is called damp green dawn, car hook, layer kettle etc., is that the Hu Guanzi of Hu Guanzi section belongs to deciduous tree.Contain higher grease (48%) in its fruit and seed, the samara oil that extracts in the samara seed has been verified therapeutic action and the oxidation resistant effect with reducing blood lipid.But the aliphatic acid of analyzing samara oil is formed and is shown, its aliphatic acid composition does not have other special composition and the aliphatic acid of common soya-bean oil is formed similar.Linolenic acid content only about 7.6% not as good as the content height of linseed oil (48%), is formed (seeing Table 1) from aliphatic acid, eats common soya-bean oil and what difference samara oil does not have.

Table 1, samara oil and soya fatty acid ratio of components are

Title	Palmitic acid	Stearic acid	Oleic acid	Linoleic acid	Leukotrienes
						Samara oil soya-bean oil	4.9 13.5	2.0 2.2	23.1 21.1	52.3 54.5	7.6 9.1

The key that this explanation samara oil plays active function is not its fatty acid composition, but its unsaponifiable matter part.After measured, the samara fat extract contains the unsaponifiable matter composition up to 10%, and wherein about 35% is phytosterol, also contains a large amount of vitamin Es or the like in addition.It is reported in the samara oil that the every 100g of natural VE content can be up to 1558.1mg, (Feng Baoying, Yang Pingying. the research of elaeagnus mollis kind Renhua analysis of components. Shanxi forestry science and technology, 1989,4 (6): 6-9).These compositions are elite parts of samara oil, can be rated as " samara essence ".

The relevant technology of extracting the samara essence (sterol thing) be rich in active material is actually rare.Ren Yinzhe (CN1068375C) discloses a kind of supercritical CO ₂The method of extraction samara oil, the separating pressure that its maximum shortcoming is overcritical separation process too low (only 100～150KPa), about 1 atmospheric pressure, can't realize the circulation and the recovery of carbon dioxide.Therefore in industrial not actual application value.Its raw material that adopts is a samara kind benevolence in addition, rather than the full fruit of samara, and it has only extracted the fatty acid composition of samara oil, and the most of phytosterols in the samara are present in parts such as pericarp.

Summary of the invention

The purpose of this invention is to provide a kind of method that from samara, prepares the samara essence that is rich in the phytosterol composition by supercritical carbon dioxide extracting.

Utilize phytosterol in supercritical fluid, to have the characteristic extracting phytosterol composition samara essence of higher solubility; By its low dissolubility property in grease, make it not only but also from grease, separate out, realize separating of phytosterol thing and grease by the centrifugal filtration means, thereby obtain to be rich in the samara essence product of phytosterol.

Purpose of the present invention realizes by following scheme:

(1). plant material samara after the drying is ground into 10-40 purpose powder, is prepared into raw meal;

(2). with the raw meal extractor of packing into, with CO ₂For carrying out grease to raw meal, extracts by extractant, control extracting pressure 15～35MPa, and temperature is at 31.1～60 ℃; The carbon dioxide that contains grease flows out from the extractor top, enters the separator decompression separation and collects separating pressure 4～10MPa, 10～80 ℃ of separation temperatures; Must contain phytosterol samara mixture;

(3). will contain phytosterol samara mixture and leave standstill precipitating at 10-25 ℃;

(4). it is centrifugal or filter to leave standstill phytosterol samara mixture after the precipitating, carries out Separation of Solid and Liquid, liquid partly samara oil, solids gets samara essence.

The present invention has following advantage:

(1) phytosterol is a liposoluble substance, easily is dissolved in the supercritical carbon dioxide fluid.Supercritical carbon dioxide fluid can more fully extract the liposoluble constituent in the raw material.Because the solubility of phytosterol samara essence in normal temperature and low temperature grease is less, can separate out from samara oil.By centrifugal, means such as filtration realized samara essence extraction and with the separating of samara oil, obtained higher degree samara essence product and samara oil, can be widely used in industries such as medical treatment, foods and cosmetics.

(2) phytosterol is contained in the exocuticle part of fruit more, plays protection seed grease.Compare with the CN1068375C patented technology, it is raw material that this method adopts the full fruit of samara, has comprised the exocuticle part, has extracted the active component of samara essence preferably, has utilized the samara raw material simultaneously to greatest extent.

(3) adopt advanced supercritical CO ₂Be green solvent, have the operating condition gentleness, free from environmental pollution, the characteristics of on-the-spot no fire hazard and product safety.

(4) when obtaining samara essence, also can obtain to be rich in the samara oil product of aliphatic acid.

(5) overcome CN1068375C patented technology separating pressure low excessively cause the carbon dioxide shortcoming that can not circulate and reclaim, reduce operating cost.

The specific embodiment

Embodiment 1:

Get the full fruit of dried samara, be ground into the 10-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor ₂The fluid extraction grease, extracting pressure 30MPa, 40 ℃ of extraction temperature, separating pressure 8MPa, 50 ℃ of separation temperatures, CO ₂7 kilograms/hour of flows, grease is separated out by separator.After 4 hours, extraction finishes, and samara oil was poured centrifuge into centrifugal 15 minutes after leaving standstill 10 hours under 15 ℃ of conditions, and solid shape thing part weighs 4.4 grams, yield 2.2%, and measuring cupreol content through the GC method is 55%, liquid partly gets samara oil.

Embodiment 2:

Get the full fruit of dried samara, be ground into the 20-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor ₂The fluid extraction grease, extracting pressure 15MPa, 60 ℃ of extraction temperature, separating pressure 9MPa, 70 ℃ of separation temperatures, CO ₂10 kilograms/hour of flows.After 6 hours, extraction finishes, and samara oil was poured centrifuge into centrifugal 20 minutes after leaving standstill 10 hours under 20 ℃ of the room temperatures, solid shape thing 3.2 grams, yield 1.6%.Measuring cupreol content through the GC method is 45%, and liquid partly gets samara oil.

Embodiment 3:

Get the full fruit of dried samara, be ground into the 10-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor ₂The fluid extraction grease, extracting pressure 32MPa, 50 ℃ of extraction temperature, separating pressure 5Mpa, 30 ℃ of separation temperatures, CO ₂7 kilograms/hour of flows extract after 4 hours and finish, and samara oil was poured centrifuge into centrifugal 15 minutes after leaving standstill 10 hours under 20 ℃ of the normal temperature, solid shape thing weigh 4.2 grams, yield 2.1%.Measuring cupreol content through the GC method is 50%, and liquid partly gets samara oil.

Embodiment 4:

Get the full fruit of dried samara, be ground into the 10-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor ₂The fluid extraction grease, extracting pressure 32MPa, 50 ℃ of extraction temperature, separating pressure 8Mpa, 40 ℃ of separation temperatures, CO ₂7 kilograms/hour of flows extract after 4 hours and finish, and samara oil was poured centrifuge into centrifugal 15 minutes after leaving standstill 10 hours under 10 ℃ of conditions, solid shape thing weigh 4 grams, yield 2.0%.Measuring cupreol content through the GC method is 40%, and liquid partly gets samara oil.

Embodiment 5:

Get the full fruit of dried samara, be ground into the 10-40 order, take by weighing raw material 200 grams, put and pass through supercritical CO in the extractor ₂The fluid extraction grease, extracting pressure 30MPa, 50 ℃ of extraction temperature, separating pressure 8Mpa, 50 ℃ of separation temperatures, CO ₂7 kilograms/hour of flows extract after 4 hours and finish, and samara oil was poured centrifuge into centrifugal 15 minutes after leaving standstill 10 hours under 25 ℃ of the normal temperature, solid shape thing weigh 3.8 grams, yield 1.9%.Measuring cupreol content through the GC method is 45%, and liquid partly gets samara oil.

Claims (1)

1, a kind of supercritical CO ₂Extract the method for samara essence, it is characterized in that comprising the steps:

(1). plant material samara after the drying is ground into 10-40 purpose powder, is prepared into raw meal;

(2). with the raw meal extractor of packing into, with CO ₂For carrying out grease to raw meal, extracts by extractant, control extracting pressure 15～35MPa, and temperature is at 31.1～60 ℃; The carbon dioxide that contains grease flows out from the extractor top, enters the separator decompression separation and collects separating pressure 4～10MPa, 10～80 ℃ of separation temperatures; Must contain phytosterol samara mixture;

(3). will contain phytosterol samara mixture and leave standstill precipitating at 10-25 ℃;

(4). it is centrifugal or filter to leave standstill phytosterol samara mixture after the precipitating, carries out Separation of Solid and Liquid, liquid partly samara oil, solids gets samara essence.