CN110724603A - Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue - Google Patents

Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue Download PDF

Info

Publication number
CN110724603A
CN110724603A CN201911018292.0A CN201911018292A CN110724603A CN 110724603 A CN110724603 A CN 110724603A CN 201911018292 A CN201911018292 A CN 201911018292A CN 110724603 A CN110724603 A CN 110724603A
Authority
CN
China
Prior art keywords
extraction
essential oil
water lily
supercritical
pigment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201911018292.0A
Other languages
Chinese (zh)
Inventor
黄秋伟
龙凌云
毛立彦
唐毓玮
檀小辉
王丽萍
唐莹莹
石兰蓉
张继
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi Subtropical Crops Research Institute
Original Assignee
Guangxi Subtropical Crops Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangxi Subtropical Crops Research Institute filed Critical Guangxi Subtropical Crops Research Institute
Priority to CN201911018292.0A priority Critical patent/CN110724603A/en
Publication of CN110724603A publication Critical patent/CN110724603A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
    • 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
    • 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
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0096—Purification; Precipitation; Filtration
    • 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
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/022—Refining
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention provides a supercritical CO of essential oil of water lily of the tropics2A process for extracting pigment from flower dregs for agricultural products includes supercritical CO extraction of water lily flower2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower to obtain the water lily essential oil; re-extracting the water lily flower dregs after oil extraction by adopting an ultrasonic-assisted solvent extraction method to obtain a pigment extract; supercritical CO used in the invention2The extraction technology for extracting the water lily essential oil can effectively improve the extraction rate of the essential oil, has no emission of extraction waste water, can extract pigment from the extracted residue without other organic solvents in a mixed way by an ultrasonic-assisted solvent extraction method so as to be applied to food industry to replace chemical synthetic additives such as chemical synthetic pigment and the like, thereby reducing the chemical additive pairsHarm to human body.

Description

Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue
Technical Field
The invention relates to the technical field of agricultural product processing, in particular to supercritical CO of essential oil of water lily of the tropics2Extraction and extraction of pigment from flower dregs.
Background
The water lily is one of world famous flowers, such as tropical red water lily, is a perennial root plant of the water lily genus of the Nymphaeaceae family, is widely distributed in tropical and temperate regions, contains rich nutritional ingredients as a medicinal and edible flower, has various physiological activities of reducing blood fat, resisting oxidation, resisting aging, enhancing immunity and the like, and has important significance for keeping human health;
the existing water lily processing and producing enterprises in China are few, the existing enterprises take water lily as a raw material to extract essential oil, the traditional steam distillation method is mainly adopted, Thailand who is the main producing country of the water lily essential oil also mainly adopts the traditional steam distillation method, but the process for extracting the flower essential oil through steam distillation is simple, the processing equipment is low in price, but the problems that the oil extraction rate is low, the extraction temperature is high, aromatic components in the extracted essential oil are easily damaged, and unpleasant odors such as cooking and the like are easily generated, so that the quality of the essential oil is reduced, the unpleasant odor of cooking can be generated in the extraction process, and other natural resources such as natural pigments and the like in processing byproducts are not completely utilized, so that the resource waste is caused and the like exist;
the method for extracting water lily essential oil by adopting a steam distillation method at present comprises the following steps: according to the material ratio of 1: 20, the crude extract is purified by adopting organic solvents such as dichloromethane and the like, and the yield of the water lily essential oil is only respectively: 0.302% of daily blossom and 0.497% of night blossom, low yield of essential oil, easy safety problem in the production operation process due to the use of organic solvent, and possible influence of environmental pollution and the like.
Therefore, how to realize the efficient extraction of the water lily essential oil, the reutilization of water lily flower residue resources and the like is urgently needed to be solved.
Disclosure of Invention
The invention aims to realize the effects of efficiently extracting water lily essential oil and recycling water lily pomace resources, and provides the supercritical CO of the tropical water lily essential oil2Extraction and extraction of pigment from flower dregs.
The invention adopts the following technical means for solving the technical problems:
the invention provides a supercritical CO of essential oil of water lily of the tropics2The extraction and pigment extraction process from flower dregs includes the following steps:
subjecting flos Nymphaeae to supercritical CO2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower to obtain the water lily essential oil;
and re-extracting the water lily flower dregs after oil extraction by adopting an ultrasonic-assisted solvent extraction method to obtain a pigment extract.
Further, supercritical CO is carried out on the water lily flowers2Before the extraction step, the method comprises the following steps:
carrying out vacuum freeze drying treatment on the water lily, and crushing and sieving the water lily.
Further, supercritical CO is carried out on the water lily flowers2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower, wherein the method further comprises the following steps:
measuring the ability of the water lily essential oil to eliminate free radicals, reduce total ability and inhibit lipid peroxidation so as to determine the oxidation resistance of the water lily essential oil.
Further, supercritical CO is carried out on the water lily flowers2Before the extraction step, the method comprises the following steps:
determining the influence of first factors such as extraction time, extraction temperature, extraction pressure, separation pressure and separation temperature on the yield of the water lily essential oil by adopting a single-factor experiment and response surface design;
subjecting the supercritical CO to the first factor2And setting the technological parameters of extraction.
Further, before the step of re-extracting the water lily flower dregs after oil extraction by adopting an ultrasonic-assisted solvent extraction method, the method comprises the following steps:
determining the influence of second factors such as ultrasonic time, ultrasonic power, material-liquid ratio, extraction time, extraction temperature, solvent concentration and the like on the yield of the water lily anthocyanidin by adopting a single-factor experiment and orthogonal experiment design;
and setting the technological parameters of the ultrasonic-assisted solvent extraction method according to the second factor.
Further, after the step of obtaining the water lily essential oil, the method further comprises the following steps:
and analyzing the chemical components of the water lily essential oil by adopting a GC-MS technology.
The invention provides supercritical CO of essential oil of water lily of the tropics2The extraction and pigment extraction process in flower residue has the following beneficial effects:
by subjecting flos Nymphaeae to supercritical CO2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower to obtain the water lily essential oil; re-extracting the water lily flower dregs after oil extraction by adopting an ultrasonic-assisted solvent extraction method to obtain a pigment extract; supercritical CO used in the invention2The extraction technology for extracting the water lily essential oil can effectively improve the extraction rate of the essential oil, has no emission of extraction waste water, can extract pigment from the extracted residue without other organic solvents in a mixed way by an ultrasonic-assisted solvent extraction method, and can be applied to food industry to replace chemical synthetic additives such as chemical synthetic pigment and the like, thereby reducing the harm of the chemical additives to human bodies.
Drawings
FIG. 1 shows supercritical CO of water lily essential oil2A flow diagram of one embodiment of the extraction and pigment extraction process in the flower residue;
FIG. 2 shows supercritical CO of water lily essential oil2Extracting anda flow diagram of a process for extracting pigment from flower residue;
FIG. 3 shows supercritical CO of essential oil of water lily in tropical zone of the invention2The essential oil obtained by extraction has the effect of eliminating DPPH free radicals;
FIG. 4 shows supercritical CO of essential oil of water lily in tropical zone of the invention2Eliminating ABTS from extracted essential oil+The effect of free radicals;
FIG. 5 shows supercritical CO of essential oil of water lily in tropical zone of the invention2The extracted essential oil has the effect of inhibiting the peroxidation of lecithin;
FIG. 6 shows supercritical CO of essential oil of water lily in tropical zone of the invention2The total reducing power capability effect of the extracted essential oil;
FIG. 7 shows supercritical CO of essential oil of water lily in tropical zone of the invention2The total antioxidant capacity effect of the extracted essential oil;
FIG. 8 shows supercritical CO of essential oil of water lily in tropical zone of the invention2And (4) extracting the obtained essential oil, and determining a total ion flow diagram by GC-MS.
The implementation, functional features and advantages of the present invention will be further described with reference to the accompanying drawings.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1 and fig. 2, a schematic flow chart of a process for extracting essential oil of water lily tropicalis by supercritical CO2 and extracting pigment from flower residue is shown respectively;
the invention provides supercritical CO of essential oil of water lily of the tropics2The extraction and pigment extraction process from flower dregs includes the following steps:
s1, supercritical CO treatment of the water lily flower2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower to obtain the water lily essential oil;
s2, re-extracting the water lily flower residue after oil extraction by adopting an ultrasonic-assisted solvent extraction method to obtain a pigment extract.
Specifically, supercritical extraction equipment, a freeze dryer, a rotary evaporator, a condensation reflux evaporator and an oven are adopted for carrying out water lily essential oil extraction and activity detection; the ultrasonic-assisted solvent extraction method is to soak the water lily flower dregs in a solvent, and simultaneously adopts ultrasonic waves for assistance to achieve the effect of extracting the pigment.
The method for extracting the essential oil from the flowers by adopting the steam distillation method has the problems of low extraction rate, unstable quality and the like, the flower residue after oil extraction is generally abandoned, the waste water also contains a large amount of organic matters, the discharge of waste residue and waste water easily causes environmental pollution, and the great waste of other effective components in the waste residue is easily caused. The invention adopts supercritical CO for the first time2The extraction technology for extracting the water lily essential oil can effectively improve the extraction rate of the essential oil, has no emission of extraction waste water, and can be used for subsequent comprehensive utilization and development without mixing other organic solvents in extracted residues, thereby achieving the purpose of environmental protection.
In a second aspect of the invention, supercritical CO is provided for water lily essential oil2The extraction and pigment extraction process in the flower residue also comprises the following steps:
raw material treatment: selecting water lily for extraction, selecting uniform and non-rotten water lily, removing impurities, and crushing to obtain water lily powder;
supercritical CO2Extracting water lily essential oil: adding water lily powder into extraction kettle, and supercritical CO2Pumping the gas into an extraction kettle under the action of a booster pump for supercritical CO2Extraction of CO2Opening the fine-tuning valve to make the CO2 fluid in supercritical state in the extraction kettle carry essential oil components into the essential oil separation kettle, and making CO in supercritical state2Transferring into gas state in the essential oil separation kettle, reducing solubility, and separating essential oil and CO2And (5) separating gas to realize extraction of essential oil.
In one embodiment, the Nymphaea tetragona is subjected to supercritical CO2Before the step S1 of extraction, the method includes:
s101, carrying out vacuum freeze drying treatment on the water lily, and crushing and sieving the water lily.
Aiming at the problems that volatile components such as essential oil are easy to volatilize, and high-temperature drying or natural air drying is easy to cause a large amount of loss of the essential oil components in the flower sample, in order to reduce the volatile loss amount of the essential oil in the flower sample in the drying process, the vacuum freeze drying technology is adopted to dry the water lily flower, so that the loss of the volatile components such as the essential oil in the flower sample can be effectively reduced.
In one embodiment, the Nymphaea tetragona is subjected to supercritical CO2After the step S1 of extracting and purifying the essential oil obtained after the extraction by a rectifying tower, the method further comprises:
s11, measuring the free radical scavenging ability, total reducing ability and lipid peroxidation inhibiting ability of the water lily essential oil to determine the oxidation resistance of the water lily essential oil.
Selecting DPPH free radical, ABTS+The elimination of 2 free radicals is used as a method for measuring the radical elimination capability of the water lily essential oil. The total reducing power is determined by potassium ferricyanide reduction. The method is used as a total antioxidant capacity determination method according to the FRAP method. The inhibition of lipid peroxidation was determined by the lecithin peroxidation inhibition method. The above measurement methods all use standard antioxidants such as ascorbic acid, rutin, BHT, etc. as control group tests.
In one example, patterns of tropical nymphaea candida presl' Baolan varieties are used as essential oil supercritical extraction materials, simultaneously, patterns with the same material level are subjected to steam distillation extraction, extraction reflux is carried out for 5 hours, water extraction essential oil is obtained, and the essential oil obtained in the two modes is used as an antioxidant activity determination raw material. Prior to determination of antioxidant activity, the test materials were divided into two groups: positive control group (ascorbic acid/VC, rutin, BHT), and test group (supercritical essential oil, water extract essential oil). Before DPPH free radical clearance rate measurement, the control group and the test group are respectively prepared into 0 by absolute ethyl alcoholThe initial concentration of each test subject was determined by conducting preliminary experiments using 5 dilutions of mg/mL, 0.10, 1.00, 10.00, and 100.00mg/mL, and setting the reaction time of the experiments to 30 min. It was found in the preliminary experiment that the control group showed a better removing effect at a concentration of 0.01mg/mL, and the test group showed a removing effect at a concentration of 1.00 mg/mL. Therefore, the control group is set to be 0.01, 0.02, 0.04, 0.06, 0.08 and 0.10mg/mL, the water lily essential oil of the test group is set to be 1.00, 2.00, 4.00, 6.00, 8.00 and 10.00mg/mL, the two concentration gradients are used as the concentration gradients for measuring the DPPH free radical scavenging capacity, and other antioxidant measurement indexes (ABTS) are used for keeping consistency+Free radical scavenging, anti-lipid peroxidation, total reducing power, total antioxidant power) are also used. From the overall assay results, the antioxidant activity of the supercritical essential oil is significantly better than that of the water-extracted essential oil, and the radical scavenging and anti-lipid peroxidation effects of the supercritical essential oil are close to those of the positive control group in the selected concentration range (fig. 3, 4 and 5), as judged by the IC50 value of the radical scavenging force: 3.855mg/mL (R)20.958) supercritical essential oil has DPPH free radical scavenging capacity equivalent to 0.011mg/mL (R)20.877 of rutin, 0.056mg/mL (R)2＝0.949)BHT；2.094mg/mL(R20.959) ABTS of supercritical essential oil+The radical scavenging capacity is equivalent to 0.023mg/mL (R)2＝0.941)VC、0.063mg/mL(R2Not equal to 0.956) rutin, 0.046mg/mL (R)20.956) BHT. The total reducing power and total antioxidant power of the supercritical essential oil are weaker than those of the positive control group (fig. 6 and 7).
In one embodiment, the Nymphaea tetragona is subjected to supercritical CO2Before the extraction step, the method comprises the following steps:
s102, determining the influence of first factors such as extraction time, extraction temperature, extraction pressure, separation pressure and separation temperature on the yield of the water lily essential oil by adopting a single-factor experiment and a response surface design;
s103, according to the first factor, the supercritical CO is processed2And setting the technological parameters of extraction.
Specifically, the above single-factor experiment and the response surface design are experiments in which a factor is defined as a variable and other factors are defined as constants so as to determine the preferable extraction time, extraction temperature, extraction pressure, separation pressure and separation temperature, and then the supercritical extraction equipment is subjected to parameter setting according to the first factor.
In some embodiments, the extraction pressure in the extraction kettle is 8-40 MPa, the extraction temperature is 35-70 ℃, and the extraction time is 0.5-3 h.
In some embodiments, the extraction pressure in the extraction kettle is 15-30 MPa, the extraction temperature is 45-60 ℃, and the extraction time is 1-2 h; preferably, the extraction pressure in the extraction kettle is 25MPa, the extraction temperature is 50 ℃, and the extraction time is 1.5 h.
In some embodiments, the water lily powder has a particle size of 10-60 mesh; preferably, the granularity of the water lily powder is 20-50 meshes; more preferably, the water lily powder has the granularity of 35 meshes.
In one embodiment, before the step of re-extracting the water lily flower dregs after oil extraction by using an ultrasonic-assisted solvent extraction method, the method comprises the following steps:
s201, determining the influence of second factors such as ultrasonic time, ultrasonic power, material-liquid ratio, extraction time, extraction temperature and solvent concentration on the yield of the water lily anthocyanidin by adopting a single-factor experiment and orthogonal experiment design;
s202, setting the technological parameters of the ultrasonic-assisted solvent extraction method according to the second factor.
Specifically, the above single-factor experiment and orthogonal experiment design are experiments in which one factor is defined as a variable and the other factors are defined as constants, so as to determine the optimal ultrasonic time, ultrasonic power, material-liquid ratio, extraction time, extraction temperature and solvent concentration, and then the parameters of the ultrasonic equipment are set according to the second factor.
In some embodiments, the ultrasonic time is 10min, the ultrasonic power is 20w, the feed-liquor ratio is 15%, the leaching time is 6h, the leaching temperature is 100 ℃, and the solvent concentration is 25%;
in some embodiments, the ultrasonic time is 15min, the ultrasonic power is 40w, the feed-liquor ratio is 30%, the leaching time is 6h, the leaching temperature is 140 ℃, and the solvent concentration is 40%;
in some embodiments, the ultrasonic time is 20min, the ultrasonic power is 60w, the feed-liquor ratio is 45%, the extraction time is 6h, the extraction temperature is 180 ℃, and the solvent concentration is 50%.
In one embodiment, after the step of obtaining the water lily essential oil, the method further comprises the following steps:
and S12, analyzing the chemical components of the water lily essential oil by adopting a GC-MS technology.
The first GC-MS detection mode is as follows:
GC conditions were as follows: rtx-5MS quartz capillary chromatography column (0.25 μm X30 m, 0.25 μm); the carrier gas is high-purity helium; the carrier gas flow is 9.5 mL/min; the sample size was 1 μ L; the split ratio is 50: 1; the temperature of a sample inlet is 250 ℃; temperature programming: the initial temperature is 40 ℃, the temperature is increased to 250 ℃ at the speed of 8 ℃/min, and the temperature is kept for 5 min;
MS conditions: the ion source is an EI source; electron energy 70 eV; the ion source temperature is 230 ℃; the interface temperature is 250 ℃; solvent delay time 3.5min, scan range m/z: 0-500, adopting full ion scanning, and obtaining the result shown in figure 8.
The second GC-MS detection mode is as follows:
the liquid sample injection mode is adopted, the sample injection amount of the water lily essential oil is 2ul, and the detection conditions are as follows: the chromatographic column is HP-5 MS; the temperature of a sample inlet is 250 ℃; the temperature rising procedure is as follows: the initial temperature is 45 ℃, the temperature is kept for 2min, then the temperature is increased to 140 ℃ at the speed of 3 ℃/min, then the temperature is increased to 200 ℃ at the speed of 6 ℃/min, and finally the temperature is increased to 260 ℃ at the speed of 6 ℃/min; the ionization mode is EI; ionization voltage 70 eV; the ion source temperature is 230 ℃; the interface temperature is 280 ℃; the detection mode is full ion scanning.
In another embodiment, before the step of performing the oxidation resistance test and the chemical composition analysis of the water lily essential oil, the method further comprises the following steps:
s3 comparative supercritical CO2The yield of the water lily essential oil obtained by extraction and steam distillation;
supercritical CO according to the comparison2The yield of the water lily essential oil obtained by extraction and steam distillation is checked to check the extraction efficiency of the supercritical CO2 extraction in the implementation process, so that the low extraction efficiency of supercritical extraction equipment is prevented.
In conclusion, the water lily is subjected to supercritical treatmentBoundary CO2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower to obtain the water lily essential oil; re-extracting the water lily flower dregs after oil extraction by adopting an ultrasonic-assisted solvent extraction method to obtain a pigment extract; supercritical CO used in the invention2The extraction technology for extracting the water lily essential oil can effectively improve the extraction rate of the essential oil, has no emission of extraction waste water, can extract pigment from the extracted residue without other organic solvents in a mixed way by an ultrasonic-assisted solvent extraction method, and can be applied to food industry to replace chemical synthetic additives such as chemical synthetic pigment and the like, thereby reducing the harm of the chemical additives to human bodies.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. Supercritical CO of essential oil of water lily of tropics2The extraction and pigment extraction process in flower residue is characterized by comprising the following steps:
subjecting flos Nymphaeae to supercritical CO2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower to obtain the water lily essential oil;
and re-extracting the water lily flower dregs after oil extraction by adopting an ultrasonic-assisted solvent extraction method to obtain a pigment extract.
2. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 12The extraction and pigment extraction process from flower residue is characterized in that supercritical CO is carried out on the water lily flower2Before the extraction step, the method comprises the following steps:
carrying out vacuum freeze drying treatment on the water lily, and crushing and sieving the water lily.
3. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 12The extraction and pigment extraction process from flower dregs is characterized by thatCharacterized in that supercritical CO is carried out on the water lily flowers2Extracting, and purifying the essential oil obtained after extraction through a rectifying tower, wherein the method further comprises the following steps:
measuring the ability of the water lily essential oil to eliminate free radicals, reduce total ability and inhibit lipid peroxidation so as to determine the oxidation resistance of the water lily essential oil.
4. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 32The extraction and pigment extraction process from flower residue is characterized in that the free radicals for measuring the scavenging capacity of the water lily essential oil on the free radicals comprise DPPH free radicals and ABTS+A free radical.
5. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 3 or 42The extraction and pigment extraction process in the flower residue comprises the following steps of:
preparing the control group and the test group into 0.01, 0.10, 1.00, 10.00 and 100.00mg/mL diluted solutions respectively by using absolute ethyl alcohol;
the 5 concentrated solutions are used for carrying out a pre-test, the reaction time of the test is 30min, so as to respectively determine a first initial concentration and a second initial concentration of the test of the control group and the test group, and the first initial concentration and the second initial concentration are used as concentration gradients for determining the DPPH free radical scavenging capacity.
6. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 12The extraction and pigment extraction process from flower residue is characterized in that supercritical CO is carried out on the water lily flower2Before the extraction step, the method comprises the following steps:
determining the influence of first factors such as extraction time, extraction temperature, extraction pressure, separation pressure and separation temperature on the yield of the water lily essential oil by adopting a single-factor experiment and response surface design;
subjecting the supercritical CO to the first factor2And setting the technological parameters of extraction.
7. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 12The extraction and pigment extraction process in flower residue is characterized in that before the step of re-extracting the water lily flower residue after oil extraction by adopting an ultrasonic-assisted solvent extraction method, the process comprises the following steps:
determining the influence of second factors such as ultrasonic time, ultrasonic power, material-liquid ratio, extraction time, extraction temperature, solvent concentration and the like on the yield of the water lily anthocyanidin by adopting a single-factor experiment and orthogonal experiment design;
and setting the technological parameters of the ultrasonic-assisted solvent extraction method according to the second factor.
8. The supercritical CO of essential oil of Nymphaea tropicalis according to claim 12The extraction and pigment extraction process in the flower residue is characterized in that after the step of obtaining the water lily essential oil, the process further comprises the following steps:
and analyzing the chemical components of the water lily essential oil by adopting a GC-MS technology.
CN201911018292.0A 2019-10-24 2019-10-24 Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue Pending CN110724603A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911018292.0A CN110724603A (en) 2019-10-24 2019-10-24 Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911018292.0A CN110724603A (en) 2019-10-24 2019-10-24 Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue

Publications (1)

Publication Number Publication Date
CN110724603A true CN110724603A (en) 2020-01-24

Family

ID=69221946

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911018292.0A Pending CN110724603A (en) 2019-10-24 2019-10-24 Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue

Country Status (1)

Country Link
CN (1) CN110724603A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111892828A (en) * 2020-09-17 2020-11-06 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） Red system Lotus subgenus water lily pigment and extraction method and application thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103537117A (en) * 2012-07-17 2014-01-29 永登苦水兴顺玫瑰花有限公司 Method for continuously and circularly extracting rose essential oil, rose juice and rose glycoside
CN104510651A (en) * 2013-09-27 2015-04-15 青岛畅绿生物研究所 Natural water lily makeup-removing massage oil
CN105860572A (en) * 2015-01-23 2016-08-17 四川大学 Method for extracting pigment, polysaccharides and flavonoids from rose dregs
CN109135931A (en) * 2018-09-04 2019-01-04 海南大学 A kind of nymphaea rubra method of extraction of essential oil
CN109401358A (en) * 2017-08-16 2019-03-01 冯顺珍 A method of haematochrome is extracted from Jasmine flower residue
CN109674693A (en) * 2017-10-18 2019-04-26 青岛正沐生物科技有限公司 A kind of Essence of the extract containing water lily and preparation method thereof
CN110205202A (en) * 2019-05-28 2019-09-06 西北农林科技大学 A kind of supercritical CO2Technique prepares the method and its technological parameter acquisition methods and peony essential oil of peony essential oil

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103537117A (en) * 2012-07-17 2014-01-29 永登苦水兴顺玫瑰花有限公司 Method for continuously and circularly extracting rose essential oil, rose juice and rose glycoside
CN104510651A (en) * 2013-09-27 2015-04-15 青岛畅绿生物研究所 Natural water lily makeup-removing massage oil
CN105860572A (en) * 2015-01-23 2016-08-17 四川大学 Method for extracting pigment, polysaccharides and flavonoids from rose dregs
CN109401358A (en) * 2017-08-16 2019-03-01 冯顺珍 A method of haematochrome is extracted from Jasmine flower residue
CN109674693A (en) * 2017-10-18 2019-04-26 青岛正沐生物科技有限公司 A kind of Essence of the extract containing water lily and preparation method thereof
CN109135931A (en) * 2018-09-04 2019-01-04 海南大学 A kind of nymphaea rubra method of extraction of essential oil
CN110205202A (en) * 2019-05-28 2019-09-06 西北农林科技大学 A kind of supercritical CO2Technique prepares the method and its technological parameter acquisition methods and peony essential oil of peony essential oil

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
刘婷，等: "水蒸气蒸馏和超临界萃取薰衣草精油抗氧化作用研究", 《时珍国医国药》 *
孙玉洁，等: "香水莲花提取物的美白功效研究", 《食品与生物技术学报》 *
邢玉娟，等: "水蒸气蒸馏和超临界萃取来凤凤菊精油抗氧化研究", 《食品研究与开发》 *
马剑忠，等: "从花瓣中提取酸碱指示剂的研究", 《科技资讯》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111892828A (en) * 2020-09-17 2020-11-06 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） Red system Lotus subgenus water lily pigment and extraction method and application thereof

Similar Documents

Publication Publication Date Title
CN102766530B (en) Method for extracting phospholipid-rich krill oil from Antarctic krill
CN106367208B (en) A kind of isolation and purification method of galic essential oil
CN103463123B (en) Method for extracting effective constituents from maca
CN101773593B (en) Method for preparing antioxidative active extractive of sweet potato leaves
CN102432582A (en) Preparation method of proanthocyanidin
CN105456155A (en) Method for preparing cosmetic raw materials from Hermetia illucens larvas and application of method
CN102166230B (en) Microwave-assisted extraction method of seaweed polyphenol
CN110724603A (en) Supercritical CO of water lily essential oil2Extraction and pigment extraction process from flower residue
CN101611878B (en) Method for preparing carotenoids in gac fruit
CN103361182B (en) Method for extraction of ginger oil by solvent
CN112778394A (en) Preparation method of rosaceous acid extract in rosa roxburghii tratt pomace
WO2017103838A1 (en) A solvent free sesamin complex 90% and a method of synthesizing the same
CN110527582A (en) A kind of consumption grease Environment-friendlyextraction extraction method
CN105085224A (en) Method of extracting hypericin from hypericum perforatum
CN111534366B (en) Method for preparing oat bran oil rich in polyphenol by taking naked oat bran as raw material
AU2020101090A4 (en) A Method for Preparing Flavonoids in Functional Passion Fruit Shells
CN104974194A (en) Technology for extracting polyphenol from grape peel residues
CN111195268A (en) Method for extracting polyphenols from pomegranate peel
CN108977269A (en) A kind of onion oil and preparation method thereof
CN111909776A (en) Method for efficiently preparing peony seed oil and obtained peony seed oil
CN105861144A (en) Supercritical extraction technology of cynomorium songaricum oil
CN106518653A (en) Membrane extraction process for hydroxycitric acid
CN110804493A (en) Extraction process of clausena lansium volatile oil
CN112920893A (en) Camellia oil and processing method thereof
CN104814505B (en) A kind of preparation method and applications of natural composite antioxidant

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination