CN106046851A - Idesia red pigments and preparation method thereof - Google Patents
Idesia red pigments and preparation method thereof Download PDFInfo
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- CN106046851A CN106046851A CN201610534890.3A CN201610534890A CN106046851A CN 106046851 A CN106046851 A CN 106046851A CN 201610534890 A CN201610534890 A CN 201610534890A CN 106046851 A CN106046851 A CN 106046851A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses idesia red pigments and a preparation method thereof. The preparation method includes the steps of firstly, preprocessing, to be more specific, removing fruit stems and mechanical impurities, and crushing and sieving to obtain processed idesia fruits; secondly, extracting, to be more specific, mixing the processed idesia fruits with petroleum ether, heating and stirring, cooling, and filtering to obtain a clear solvent; thirdly, removing the solvent, to be more specific, performing pressure-reduced distillation on the clear solvent to obtain idesia oil containing the red pigments; fourthly, performing macroporous resin separation, to be more specific, adding the idesia oil containing the red pigments into weak-polarity macroporous resin for standing and absorption, leaching the weak-polarity macroporous resin with ethyl acetate until leachate is not red, and performing pressure-reduced distillation on the ethyl acetate leachate to obtain oily substances; fifthly, performing molecular distillation separation, to be more specific, distilling the oily substances in a molecular distillation instrument to obtain the idesia red pigments. The idesia red pigments prepared by the method is resistant to strong light irradiation and oxidization.
Description
Technical field
The present invention relates to a kind of Radix seu Cortex Malloti nepalensis red pigment and preparation method thereof.
Background technology
Radix seu Cortex Malloti nepalensis is Flacourtiaceae plant, and produced fruit is the woody oleiferous plants that a kind of oil content is the highest.Radix seu Cortex Malloti nepalensis fruit squeezes
The oily unsaturated fatty acids content gone out is high, and wherein linoleic acid content reaches more than 60%, is the edible oil of a kind of rich in nutritive value.
Containing a kind of red pigment in Radix seu Cortex Malloti nepalensis fruit, presenting shiny red, oil-soluble is strong, good stability in oils and fats, for a long time
It is exposed under air, high light colour-fast, is the natural pigment of a kind of function admirable.
At present, in food, the pigment of application includes two kinds: natural pigment and synthetic food color.Along with people are to food
The growing interest of safety problem, natural pigment is becoming increasingly popular.But, the red pigment in Radix seu Cortex Malloti nepalensis fruit does not cause pass
Note, had carried out the research of removing by red pigment during the most only people mentions prepared Radix seu Cortex Malloti nepalensis oil product.The present invention utilizes molecule
Radix seu Cortex Malloti nepalensis red pigment is prepared in distillation technique and low pole macroporous adsorbent resin combination.
Summary of the invention
It is an object of the invention to a kind of Radix seu Cortex Malloti nepalensis red pigment of providing for making full use of red pigment in Radix seu Cortex Malloti nepalensis fruit and
Its preparation method, the feature of described preparation method is to use molecular distillation technique and low pole macroporous adsorbent resin combination preparation mountain
Seeds of a tung oil tree red pigment.
The purpose of the present invention is realized by techniques below, and wherein, described raw material number is parts by weight, unless otherwise rule
Fixed.
According to an aspect of the present invention, the present invention provides the preparation method of a kind of Radix seu Cortex Malloti nepalensis red pigment, comprises the following steps:
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60
Eye mesh screen, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process is mixed, heats and stir institute with certain number petroleum ether
State mixture, be cooled to room temperature and filter to remove filtering residue, obtain settled solution;
3) desolvation: under uniform temperature and pressure, described settled solution is carried out decompression distillation thus removes in solvent
Component in addition to red pigment with idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added certain number low pole big
Standing adsorption certain time in macroporous adsorbent resin, have no to leacheate with low pole macroporous adsorbent resin described in ethyl acetate drip washing
Red, again with low pole macroporous adsorbent resin described in petroleum ether drip washing, under uniform temperature and pressure, petroleum ether leacheate is entered
Row decompression distillation distillates to solvent-free, obtains colourless idesia oil.Further, to ethyl acetate drip washing under uniform temperature and pressure
Liquid carries out decompression distillation and distillates to solvent-free, obtains grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, distills under certain condition, obtain
Paste i.e. Radix seu Cortex Malloti nepalensis red pigment,
Wherein, described low pole macroporous adsorbent resin is AD-8 type.
According to the embodiment of the present invention,
In described step 2) in, described petroleum ether number can be 140-160 part, and described heating-up temperature can be 45-65
DEG C, described mixing time can be 60-120 minute;
In described step 3) in, described pressure can be 0.4-0.8MPa, and described heating-up temperature can be 40-60 DEG C;
In described step 4) in, described resin number can be 40-50 part, and described adsorption time can be 40-70 minute,
Pressure in described petroleum ether leacheate can be 0.4-0.8MPa, and in described petroleum ether leacheate, heating-up temperature can be 40-
60 DEG C, the pressure in described ethyl acetate leacheate can be 0.4-0.8MPa, heating-up temperature in described ethyl acetate leacheate
Can be 50-70 DEG C;
In described step 5) in, described molecular distillation instrument flow velocity can be 2-5ml/min, and described scraper plate rotating speed can be
120-420 turns/min, and described temperature can be 110-120 DEG C, and described pressure can be 1-10Pa.
According to the embodiment of the present invention, it is preferable that
In described step 2) in, described petroleum ether number is 150 parts, and described heating-up temperature is 55 DEG C, described mixing time
It it is 90 minutes;
In described step 3) in, described pressure is 0.6MPa, and described heating-up temperature is 50 DEG C;
In described step 4) in, described resin number is 45 parts, and described adsorption time is 45-55 minute, described petroleum ether
Pressure in leacheate is 0.5-0.7MPa, and in described petroleum ether leacheate, heating-up temperature is 45-55 DEG C, and described ethyl acetate is drenched
Pressure in washing liquid is 0.5-0.7MPa, and in described ethyl acetate leacheate, heating-up temperature is 55-65 DEG C;
In described step 5) in, described molecular distillation instrument flow velocity is 3-4ml/min, described scraper plate rotating speed be 200-350 turn/
Min, described temperature is 113-116 DEG C, and described pressure is 3-6Pa.
According to the embodiment of the present invention, it is highly preferred that
In described step 2) in, described petroleum ether number is 150 parts, and described heating-up temperature is 55 DEG C, described mixing time
It it is 90 minutes;
In described step 3) in, described pressure is 0.6MPa, and described heating-up temperature is 50 DEG C;
In described step 4) in, described resin number is 45 parts, and described adsorption time is 50 minutes, described petroleum ether drip washing
Pressure in liquid is 0.6MPa, and in described petroleum ether leacheate, heating-up temperature is 50 DEG C, the pressure in described ethyl acetate leacheate
Power is 0.6MPa, and heating-up temperature described in ethyl acetate leacheate is 60 DEG C;
In described step 5) in, described molecular distillation instrument flow velocity is 3.5ml/min, and described scraper plate rotating speed is 270 turns/min,
Described temperature is 115 DEG C, and described pressure is 5Pa.
According to the embodiment of the present invention, described preparation method can obtain Radix seu Cortex Malloti nepalensis red pigment and colourless idesia oil.
According to the embodiment of the present invention, described Radix seu Cortex Malloti nepalensis red pigment can be applied in food.
According to an aspect of the present invention, the present invention provides the Radix seu Cortex Malloti nepalensis red pigment obtained by above-mentioned preparation method.
Performance test: measure described mountain paulownia with UV2600 type ultraviolet spectrophotometer (Shanghai You Nike Instrument Ltd.)
The color valency of sub-red pigment, uses standard GB/T 15961-2005 that described Radix seu Cortex Malloti nepalensis red pigment carries out color valency mensuration and color valency meter
Calculate.
The present invention has the following advantages.
Use Radix seu Cortex Malloti nepalensis red pigment stable in properties prepared by described preparation method, be a kind of resistance to strong illumination, sludge proof
Natural pigment, additionally, the preparation method of the present invention is simple, technological process is short, and can obtain simultaneously colourless idesia oil and
Radix seu Cortex Malloti nepalensis red pigment.
Detailed description of the invention
Below in conjunction with embodiment, it is more fully described the detailed description of the invention of the present invention.Following example are merely to illustrate
Purpose and do not limit the scope of the invention.
Embodiment 1
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60
Eye mesh screen, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process and 140 parts of petroleum ether are mixed, added by described mixture
Heat to 45 DEG C, stirring 60 minutes, be cooled to room temperature and filter filtering residue, obtain settled solution;
3) desolvation: described settled solution is heated under 0.4MPa 40 DEG C of decompression distillations thus removes in solvent and remove
Component outside red pigment and idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added 40 parts of AD-8 type low poles
In macroporous adsorbent resin, standing adsorption 40 minutes, use ethyl acetate drip washing AD-8 type low pole macroporous adsorbent resin are to leacheate not
Show color, again with petroleum ether drip washing AD-8 type low pole macroporous adsorbent resin, petroleum ether leacheate is heated under 0.4MPa
40 DEG C of decompression distillations distillate to solvent-free, obtain colourless idesia oil.Ethyl acetate leacheate is heated to 50 DEG C under 0.4MPa
Decompression distillation distillates to solvent-free, obtains grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, is 2ml/ at molecular distillation instrument flow velocity
Min, scraper plate rotating speed are 120 turns/min, temperature is 110 DEG C, pressure is to distill under conditions of 1Pa, obtained paste
I.e. Radix seu Cortex Malloti nepalensis red pigment.
Embodiment 2
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60
Eye mesh screen, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process and 160 parts of petroleum ether are mixed, added by described mixture
Heat to 65 DEG C, stirring 120 minutes, be cooled to room temperature and filter filtering residue, obtain settled solution;
3) desolvation: described settled solution is heated under 0.8MP 60 DEG C of decompression distillations thus removes in solvent and remove
Component outside red pigment and idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added 50 parts of AD-8 type low poles
In macroporous adsorbent resin, standing adsorption 70 minutes, use ethyl acetate drip washing AD-8 type low pole macroporous adsorbent resin are to leacheate not
Show color, again with petroleum ether drip washing AD-8 type low pole macroporous adsorbent resin, petroleum ether leacheate is heated under 0.8MPa
60 DEG C of decompression distillations distillate to solvent-free, obtain colourless idesia oil.Ethyl acetate leacheate is heated to 70 DEG C under 0.8MPa
Decompression distillation distillates to solvent-free, obtains grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, is 5ml/ at molecular distillation instrument flow velocity
Min, scraper plate rotating speed are 420 turns/min, temperature is 120 DEG C, pressure is to distill under conditions of 10Pa, obtained paste
I.e. Radix seu Cortex Malloti nepalensis red pigment.
Embodiment 3
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60
Eye mesh screen, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process and 150 parts of petroleum ether are mixed, added by described mixture
Heat to 55 DEG C, stirring 90 minutes, be cooled to room temperature and filter filtering residue, obtain settled solution;
3) desolvation: described settled solution is heated under 0.6MPa 50 DEG C of decompression distillations thus removes in solvent and remove
Component outside red pigment and idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added 45 parts of AD-8 type low poles
In macroporous adsorbent resin, standing adsorption 55 minutes, use ethyl acetate drip washing AD-8 type low pole macroporous adsorbent resin are to leacheate not
Show color, again with petroleum ether drip washing AD-8 type low pole macroporous adsorbent resin, petroleum ether leacheate is heated under 0.6MPa
50 DEG C of decompression distillations distillate to solvent-free, obtain colourless idesia oil.Ethyl acetate leacheate is heated to 60 DEG C under 0.6MPa
Decompression distillation distillates to solvent-free, obtains grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, is 3.5ml/ at molecular distillation instrument flow velocity
Min, scraper plate rotating speed are 270 turns/min, temperature is 115 DEG C, pressure is to distill under conditions of 5Pa, obtained paste
I.e. Radix seu Cortex Malloti nepalensis red pigment.
Embodiment 4
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60
Eye mesh screen, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process and 150 parts of petroleum ether are mixed, added by described mixture
Heat to 55 DEG C, stirring 90 minutes, be cooled to room temperature and filter filtering residue, obtain settled solution;
3) desolvation: described settled solution is heated under 0.6MPa 50 DEG C of decompression distillations thus removes in solvent and remove
Component outside red pigment and idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added 45 parts of AD-8 type low poles
In macroporous adsorbent resin, standing adsorption 65 minutes, use ethyl acetate drip washing AD-8 type low pole macroporous adsorbent resin are to leacheate not
Show color, again with petroleum ether drip washing AD-8 type low pole macroporous adsorbent resin, petroleum ether leacheate is heated under 0.7MPa
55 DEG C of decompression distillations distillate to solvent-free, obtain colourless idesia oil.Ethyl acetate leacheate is heated to 65 DEG C under 0.7MPa
Decompression distillation distillates to solvent-free, obtains grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, is 4ml/ at molecular distillation instrument flow velocity
Min, scraper plate rotating speed are 350 turns/min, temperature is 116 DEG C, pressure is to distill under conditions of 6Pa, obtained paste
I.e. Radix seu Cortex Malloti nepalensis red pigment.
Embodiment 5
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60
Eye mesh screen, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process and 150 parts of petroleum ether are mixed, added by described mixture
Heat to 55 DEG C, stirring 90 minutes, be cooled to room temperature and filter filtering residue, obtain settled solution;
3) desolvation: described settled solution is heated under 0.6MP 50 DEG C of decompression distillations thus removes in solvent and remove
Component outside red pigment and idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added 45 parts of AD-8 type low poles
In macroporous adsorbent resin, standing adsorption 45 minutes, use ethyl acetate drip washing AD-8 type low pole macroporous adsorbent resin are to leacheate not
Show color, again with petroleum ether drip washing AD-8 type low pole macroporous adsorbent resin, petroleum ether leacheate is heated under 0.5MPa
45 DEG C of decompression distillations distillate to solvent-free, obtain colourless idesia oil.Ethyl acetate leacheate is heated to 55 DEG C under 0.5MPa
Decompression distillation distillates to solvent-free, obtains grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, is 3ml/ at molecular distillation instrument flow velocity
Min, scraper plate rotating speed are 200 turns/min, temperature is 113 DEG C, pressure is to distill under conditions of 3Pa, obtained paste
I.e. Radix seu Cortex Malloti nepalensis red pigment.
Embodiment 1,2,3,4,5 is analyzed, obtains Radix seu Cortex Malloti nepalensis red pigment product and the index of technique, as shown in table 1.
Table 1
By table 1 it can be concluded that
(1) the color valency of the product of embodiment 2,3,4 preparation is higher, and the color valency of the product of embodiment 1 preparation is the highest.
(2) the selection process index in embodiment is as follows:
In step 2) in, petroleum ether number is 150 parts, and heating-up temperature is 55 DEG C, and mixing time is 90 minutes,
In step 3) in, pressure is 0.6MPa, and heating-up temperature is 50 DEG C,
In step 4) in, resin number is 45 parts, and adsorption time is 45-55 minute, and the pressure in petroleum ether leacheate is
0.5-0.7MPa, in petroleum ether leacheate, heating-up temperature is 45-55 DEG C, and the pressure in ethyl acetate leacheate is 0.5-
0.7MPa, in ethyl acetate leacheate, heating-up temperature is 55-65 DEG C,
In step 5) in, molecular distillation instrument flow velocity is 3-4ml/min, and scraper plate rotating speed is that 200-350 turns/min, and temperature is
113-116 DEG C, pressure is 3-6Pa.
(3) the more preferably technic index in embodiment is as follows:
In step 2) in, petroleum ether number is 150 parts, and heating-up temperature is 55 DEG C, and mixing time is 90 minutes,
In step 3) in, pressure is 0.6MPa, and heating-up temperature is 50 DEG C,
In step 4) in, resin number is 45 parts, and adsorption time is 50 minutes, and the pressure in petroleum ether leacheate is
0.6MPa, in petroleum ether leacheate, heating-up temperature is 50 DEG C, and the pressure in ethyl acetate leacheate is 0.6MPa, and ethyl acetate is drenched
In washing liquid, heating-up temperature is 60 DEG C,
In step 5) in, molecular distillation instrument flow velocity is 3.5ml/min, and scraper plate rotating speed is 270 turns/min, and temperature is 115 DEG C,
Pressure is 5Pa.
Claims (8)
1. a preparation method for Radix seu Cortex Malloti nepalensis red pigment, comprises the following steps:
1) pretreatment: reject raw material goes rotten Radix seu Cortex Malloti nepalensis fruit, remove fruit stem and mechanical admixture, pulverize and cross 40-60 mesh sieve
Net, the Radix seu Cortex Malloti nepalensis fruit after being processed;
2) extraction: the Radix seu Cortex Malloti nepalensis fruit after 100 parts of described process is mixed, heats and stirs described mixed with certain number petroleum ether
Compound, it is cooled to room temperature and filters to remove filtering residue, obtaining settled solution;
3) desolvation: under uniform temperature and pressure, described settled solution is carried out decompression distillation thus remove in solvent except
Component outside red pigment and idesia oil, obtains the idesia oil containing red pigment after cooling;
4) macroporous adsorbent resin separates: the idesia oil containing red pigment described in 100 parts is added certain number low pole macropore and inhales
In attached resin, low pole macroporous adsorbent resin described in standing adsorption certain time, use ethyl acetate drip washing is to the non-show of leacheate
Color, again with low pole macroporous adsorbent resin described in petroleum ether drip washing, under uniform temperature and pressure, petroleum ether leacheate is carried out
Decompression distillation distillates to solvent-free, obtains colourless idesia oil.Further, to ethyl acetate leacheate under uniform temperature and pressure
Carry out decompression distillation to distillate to solvent-free, obtain grease;With
5) molecular distillation separates: is added in molecular distillation instrument by described grease, distills under certain condition, the cream obtained
Shape thing i.e. Radix seu Cortex Malloti nepalensis red pigment,
Wherein, described low pole macroporous adsorbent resin is AD-8 type.
Preparation method the most according to claim 1, wherein,
In described step 2) in, described petroleum ether number is 140-160 part, and described heating-up temperature is 45-65 DEG C, during described stirring
Between be 60-120 minute,
In described step 3) in, described pressure is 0.4-0.8MPa, and described heating-up temperature is 40-60 DEG C,
In described step 4) in, described resin number is 40-50 part, and described adsorption time is 40-70 minute, and described petroleum ether drenches
Pressure in washing liquid is 0.4-0.8MPa, and in described petroleum ether leacheate, heating-up temperature is 40-60 DEG C, described ethyl acetate drip washing
Pressure in liquid is 0.4-0.8MPa, and in described ethyl acetate leacheate, heating-up temperature is 50-70 DEG C,
In described step 5) in, described molecular distillation instrument flow velocity is 2-5ml/min, and described scraper plate rotating speed is that 120-420 turns/min,
Described temperature is 110-120 DEG C, and described pressure is 1-10Pa.
Preparation method the most according to claim 2, wherein,
In described step 2) in, described petroleum ether number is 150 parts, and described heating-up temperature is 55 DEG C, and described mixing time is 90
Minute,
In described step 3) in, described pressure is 0.6MPa, and described heating-up temperature is 50 DEG C,
In described step 4) in, described resin number is 45 parts, and described adsorption time is 45-55 minute, described petroleum ether drip washing
Pressure in liquid is 0.5-0.7MPa, and in described petroleum ether leacheate, heating-up temperature is 45-55 DEG C, described ethyl acetate leacheate
In pressure be 0.5-0.7MPa, in described ethyl acetate leacheate, heating-up temperature is 55-65 DEG C,
In described step 5) in, described molecular distillation instrument flow velocity is 3-4ml/min, and described scraper plate rotating speed is that 200-350 turns/min,
Described temperature is 113-116 DEG C, and described pressure is 3-6Pa.
Preparation method the most according to claim 3, wherein,
In described step 2) in, described petroleum ether number is 150 parts, and described heating-up temperature is 55 DEG C, and described mixing time is 90
Minute,
In described step 3) in, described pressure is 0.6MPa, and described heating-up temperature is 50 DEG C,
In described step 4) in, described resin number is 45 parts, and described adsorption time is 50 minutes, in described petroleum ether leacheate
Pressure be 0.6MPa, in described petroleum ether leacheate, heating-up temperature is 50 DEG C, and the pressure in described ethyl acetate leacheate is
0.6MPa, heating-up temperature described in ethyl acetate leacheate is 60 DEG C,
In described step 5) in, described molecular distillation instrument flow velocity is 3.5ml/min, and described scraper plate rotating speed is 270 turns/min, described
Temperature is 115 DEG C, and described pressure is 5Pa.
Preparation method the most according to claim 1, wherein, described preparation method obtains Radix seu Cortex Malloti nepalensis red pigment and colourless mountain paulownia
Seed oil.
Preparation method the most according to claim 1, wherein, described Radix seu Cortex Malloti nepalensis red pigment is applied in food.
7. the Radix seu Cortex Malloti nepalensis red pigment obtained according to the preparation method described in any one in claim 1-6.
Radix seu Cortex Malloti nepalensis red pigment the most according to claim 7, it is applied in food.
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CN109735133A (en) * | 2019-02-18 | 2019-05-10 | 华中农业大学 | The separation method of pigment in a kind of idesia oil |
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