CN108315098A - A kind of Nymphaea caerulea method of extraction of essential oil and its application - Google Patents

A kind of Nymphaea caerulea method of extraction of essential oil and its application Download PDF

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Publication number
CN108315098A
CN108315098A CN201810208249.XA CN201810208249A CN108315098A CN 108315098 A CN108315098 A CN 108315098A CN 201810208249 A CN201810208249 A CN 201810208249A CN 108315098 A CN108315098 A CN 108315098A
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China
Prior art keywords
essential oil
extraction
nymphaea caerulea
nymphaea
caerulea
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CN201810208249.XA
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Chinese (zh)
Inventor
赵莹
王健
宋希强
余文刚
范杨杨
吉浩
鹿文举
柏宝冰
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Hainan University
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Hainan University
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction

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

Abstract

The invention belongs to from raw materials recovery or refined essential oil technical field, disclose a kind of Nymphaea caerulea method of extraction of essential oil and its application, steam distillation and solvent extraction are combined together by straightforward procedure, the concentration of fragrance ingredient and separation are combined into one, reduce experimental procedure, easy to operate, qualitative, quantitative effect is good;Micro ingredient can be concentrated thousands of times with less solvent, it is higher to flavor component extraction efficiency, and it is avoided that the negative effect for being heated at high temperature bring for a long time.The present invention therefrom extracts essential oil using Nymphaea caerulea petal as raw material, using Simultaneous distillation (SDE), then identifies the main chemical compositions in essential oil by GC MS means, and carries out Primary Study to the in vitro anti-oxidation of essential oil.

Description

A kind of Nymphaea caerulea method of extraction of essential oil and its application
Technical field
The invention belongs to from raw materials recovery or refined essential oil technical field more particularly to a kind of Nymphaea caerulea extraction of essential oil side Method and its application.
Background technology
Currently, the prior art commonly used in the trade is such:Nymphaea (Nymphaea) is Nymphaeceae (Nymphaeaceae) there is extensive plantation in perennial aquatic herbaceous plant in temperate zone and torrid areas.Nymphaea tetragona ornamental, root Shape stem can cook.Modern research shows that water lily platymiscium contains multiple types compound, such as flavones, polysaccharide and alkaloid etc.. It isolates to obtain flavonoids from water lily platymiscium and phenolic acid compound more than 70 is planted, respectively flavones, flavonols and isoflavones Class.Water lily platymiscium has long medicinal history civil, and wherein Nymphaea candida flower (Nymphaea candida) is China The traditional medicine of the Uygur nationality people, its dry flower have been incorporated into《Drug Standard of Ministry of Public Health of the Peoples Republic of China ties up me That medicine fascicle》In, the treatment for illnesss such as cat fever, headache cough, palpitation and restlessness, pharyngalgia.According to the nutrition to water lily Constituent analysis, the results showed that water lily is rich in 17 kinds of amino acid, water lily albumen category high-quality protein.Analysis result also shows that water lily contains Abundant VC, glycosides displayed, trace element zinc, both cooperation have very strong lead-expelling function.Water lily passes through animal acute toxicity The safety evaluatios such as experiment, micronucleus test and semen teraogenesis test, all show that its safety is higher.Currently, from various plants Internal isolated extraction of essential oil object, such as rose, arborvitae, peanut, folium artemisiae argyi, but China mainly concentrates the research of Nymphaea caerulea In gardening and breeding etc., Nymphaea caerulea essential oil extracts general or traditional steam distillation, organic solvent extractionprocess And supercritical CO2Extraction, wherein steam distillation used time are longer, and volatile oil is easy to decompose at high temperature;Organic solvent The essential oil impurity that extraction obtains is more and essential oil yield is relatively low;Supercritical carbon dioxide fluid extraction is more demanding to experimental facilities, investment compared with Greatly.
In conclusion problem of the existing technology is:
(1) the steam distillation used time is longer, and volatile oil is easy to decompose at high temperature;
(2) the essential oil impurity that organic solvent extractionprocess obtains is more and essential oil yield is relatively low;
(3) supercritical CO2Extraction is more demanding to experimental facilities, and investment is larger;
Solve the difficulty and meaning of above-mentioned technical problem:Difficulty is that experiment condition or equipment requirement are higher, experimental method It is undesirable, it only lowers the requirement in conjunction with other cofactors, improves experimental method, extraction efficiency and yield could be improved.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of Nymphaea caerulea method of extraction of essential oil and its applications.
The invention is realized in this way a kind of Nymphaea caerulea method of extraction of essential oil, the Nymphaea caerulea method of extraction of essential oil is with indigo plant Water lily petal is raw material, and essential oil is extracted using Simultaneous distillation;Steam distillation and solvent extraction are passed through into straightforward procedure It is combined together, the concentration of fragrance ingredient and separation is combined into one.
Steam distillation and solvent extraction are carried out at the same time on distillation extraction instrument at the same time, it is not necessary to be collected a large amount of vapor and be distillated Liquid need not also extract vapor distillate using a large amount of organic solvents, and a large amount of organic extract liquids obtained are carried out Concentration.Through Simultaneous distillation-extraction instrument processing after, directly obtain volatility, half volatile organic solvent concentrate.It distills simultaneously Extraction simplifies experimental procedure, reduces workload, and organic solvent is greatly saved, and shortens analysis time.
Further, the Nymphaea caerulea method of extraction of essential oil includes the following steps:
Step 1, the dissociation of Nymphaea caerulea petal crush at 50 DEG C after dry 10h, cross 60 mesh and sieve to obtain Nymphaea caerulea flower Valve powder;
Step 2 is carried under the conditions of different NaCl contents, distillation time and solid-liquid ratio respectively using Simultaneous distillation Take essential oil.
Another object of the present invention is to provide a kind of Nymphaea caerulea essential oil obtained by the Nymphaea caerulea method of extraction of essential oil, The Nymphaea caerulea essential oil main component is carbonyl complex.
In conclusion advantages of the present invention and good effect are:Steam distillation is common extraction of essential oil method, production Object fragrance is more true to nature, but extraction efficiency is relatively low, and heating time is longer in production process, be easy to cause boiling breath.Together When Water distillation extractor steam distillation and solvent extraction are combined together by straightforward procedure, by the concentration of fragrance ingredient and point From being combined into one, reduce experimental procedure, easy to operate, qualitative, quantitative effect is good;It can be with less solvent by micro ingredient Thousands of times of concentration, it is higher to flavor component extraction efficiency, and it is avoided that the negative effect for being heated at high temperature bring for a long time.The present invention Using Nymphaea caerulea petal as raw material, essential oil is therefrom extracted using Simultaneous distillation (SDE), then essence is identified by GC-MS means Main chemical compositions in oil, and Primary Study is carried out to the in vitro anti-oxidation of essential oil.
Three kinds of method of extraction of essential oil compare
Description of the drawings
Fig. 1 is Nymphaea caerulea method of extraction of essential oil flow chart provided in an embodiment of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Water lily pollen is full of nutrition, has the characteristics that completeness, harmony, concentration property, has exploitation prospect Natural nutrition source.Therefore, it has broad application prospects in food, medical and health and cosmetic industry.
As shown in Figure 1, Nymphaea caerulea method of extraction of essential oil provided in an embodiment of the present invention includes the following steps:
S101:Nymphaea caerulea petal dissociates, and at 50 DEG C after dry 10h, crushes, and crosses 60 mesh and sieves to obtain Nymphaea caerulea petal Powder;
S102:Using Simultaneous distillation, extracted under the conditions of different NaCl contents, distillation time and solid-liquid ratio respectively Essential oil.
The application effect of the present invention is explained in detail with reference to experiment.
Prepared by the Nymphaea caerulea petal powder of the present invention and different factors prepare Nymphaea caerulea essential oil to Simultaneous distillation and obtain The influence of rate.Nymphaea caerulea petal is dissociated, at 50 DEG C after dry 10h, is crushed, 60 mesh is crossed and sieves to obtain Nymphaea caerulea petal powder End.Then Simultaneous distillation is used, extracts essential oil under the conditions of different NaCl contents, distillation time and solid-liquid ratio respectively, Using essential oil yield as inspection target.The results show that in 10%NaCl contents, essential oil yield highest is 0.14%;It is distilling When 4h, essential oil yield highest is 0.16%;It is 1 in solid-liquid ratio:When 20, essential oil yield highest is 0.10%.
Constituent analysis is carried out to Nymphaea caerulea essential oil using GC/MS combined instruments, main component is some carbonyl complexs, such as 2- heptadecanones, also alkenes compounds, such as phytol.
Study on Its Antioxidant Activity in Vitro mainly removes DPPH and ABTS determining free radicals.Two kinds of Nymphaea caerulea essential oil pair is certainly Increased with its concentration by the clearance rate of base and is increased.Experiment shows that Nymphaea caerulea essential oil has certain in vitro anti-oxidation, but It is that inoxidizability ratio BHT is weak.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1:Accurately weigh 30g Nymphaea caerulea petal powder.It is positioned in 1L flasks, with 600mL 5%NaCl solution Petal powder is impregnated, 4h is standing and soak for, is installed on the left end of SDE method, its boiling is heated to electric jacket It rises;100mL dichloromethane is packed into the flask of 500mL, the right end of SDE method is accessed, is heated with thermostat water bath Make its boiling to 50 DEG C.After Simultaneous distillation-extraction 2h, the flask that right end is equipped with dichloromethane is removed, anhydrous sodium sulfate is added and carries out Dry, rotary evaporation removes organic reagent, obtains essential oil product, and it is 0.10% to calculate yield.
Embodiment 2:Accurately weigh 30g Nymphaea caerulea petal powder.It is positioned in 1L flasks, with 600mL10%NaCl solution Petal powder is impregnated, 4h is standing and soak for, is installed on the left end of SDE method, its boiling is heated to electric jacket It rises;100mL dichloromethane is packed into the flask of 500mL, the right end of SDE method is accessed, is heated with thermostat water bath Make its boiling to 50 DEG C.After Simultaneous distillation-extraction 2h, the flask that right end is equipped with dichloromethane is removed, anhydrous sodium sulfate is added and carries out Dry, rotary evaporation removes organic reagent, obtains essential oil product, and it is 0.14% to calculate yield.
Embodiment 3:30g Nymphaea caerulea petal powder accurately is weighed, is positioned in 1L flasks, with 600mL10%NaCl solution Petal powder is impregnated, 4h is standing and soak for, is installed on the left end of SDE method, its boiling is heated to electric jacket It rises;100mL dichloromethane is packed into the flask of 500mL, the right end of SDE method is accessed, is heated with thermostat water bath Make its boiling to 50 DEG C.After Simultaneous distillation-extraction 4h, the flask that right end is equipped with dichloromethane is removed, anhydrous sodium sulfate is added and carries out Dry, rotary evaporation removes organic reagent, obtains essential oil product, and it is 0.16% to calculate yield.
Embodiment 4:30g Nymphaea caerulea petal powder accurately is weighed, is positioned in 1L flasks, with 600mL10%NaCl solution Petal powder is impregnated, 4h is standing and soak for, is installed on the left end of SDE method, its boiling is heated to electric jacket It rises;100mL dichloromethane is packed into the flask of 500mL, the right end of SDE method is accessed, is heated with thermostat water bath Make its boiling to 50 DEG C.After Simultaneous distillation-extraction 5h, the flask that right end is equipped with dichloromethane is removed, anhydrous sodium sulfate is added and carries out Dry, rotary evaporation removes organic reagent, obtains essential oil product, and it is 0.12% to calculate yield.
Embodiment 5:30g Nymphaea caerulea petal powder accurately is weighed, is 1 with solid-liquid ratio:20 leaching of aqueous solution containing 10%NaCl Flower bulb valve powder, is standing and soak for 4h, is installed on the left end of SDE method, its boiling is heated to electric jacket; 100mL dichloromethane is packed into the flask of 500mL, the right end of SDE method is accessed, is heated to thermostat water bath 50 DEG C make its boiling.After Simultaneous distillation-extraction 4h, the flask that right end is equipped with dichloromethane is removed, anhydrous sodium sulfate is added and is done Dry, rotary evaporation removes organic reagent, obtains essential oil product, and it is 0.11% to calculate yield.
Embodiment 6:30g Nymphaea caerulea petal powder accurately is weighed, is 1 with solid-liquid ratio:25 leaching of aqueous solution containing 10%NaCl Flower bulb valve powder, is standing and soak for 4h, is installed on the left end of SDE method, its boiling is heated to electric jacket; 100mL dichloromethane is packed into the flask of 500mL, the right end of SDE method is accessed, is heated to thermostat water bath 50 DEG C make its boiling.After Simultaneous distillation-extraction 4h, the flask that right end is equipped with dichloromethane is removed, anhydrous sodium sulfate is added and is done Dry, rotary evaporation removes organic reagent, obtains essential oil product, and it is 0.08% to calculate yield.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.

Claims (3)

1. a kind of Nymphaea caerulea method of extraction of essential oil, which is characterized in that the Nymphaea caerulea method of extraction of essential oil is with Nymphaea caerulea petal Raw material extracts essential oil using Simultaneous distillation;Steam distillation and solvent extraction are combined together by straightforward procedure, The concentration of fragrance ingredient and separation are combined into one.
2. Nymphaea caerulea method of extraction of essential oil as described in claim 1, which is characterized in that the Nymphaea caerulea method of extraction of essential oil packet Include following steps:
Step 1, the dissociation of Nymphaea caerulea petal crush at 50 DEG C after dry 10h, cross 60 mesh and sieve to obtain Nymphaea caerulea petal powder End;
Step 2 extracts essence under the conditions of different NaCl contents, distillation time and solid-liquid ratio respectively using Simultaneous distillation Oil.
3. a kind of Nymphaea caerulea essential oil that the Nymphaea caerulea method of extraction of essential oil described in claim 1 obtains, which is characterized in that the indigo plant Water lily essential oil main component is carbonyl complex.
CN201810208249.XA 2018-03-14 2018-03-14 A kind of Nymphaea caerulea method of extraction of essential oil and its application Pending CN108315098A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN109135931A (en) * 2018-09-04 2019-01-04 海南大学 A kind of nymphaea rubra method of extraction of essential oil
CN110055132A (en) * 2019-03-28 2019-07-26 广州白云山维一实业股份有限公司 The method of purification of plants essential oil
CN112481035A (en) * 2020-11-18 2021-03-12 河北中烟工业有限责任公司 Extraction method of fresh lotus essential oil
CN113439834A (en) * 2020-03-25 2021-09-28 广东省禾基生物科技有限公司 Preparation method of water lily flower cell water and application of water lily flower cell water

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109135931A (en) * 2018-09-04 2019-01-04 海南大学 A kind of nymphaea rubra method of extraction of essential oil
CN110055132A (en) * 2019-03-28 2019-07-26 广州白云山维一实业股份有限公司 The method of purification of plants essential oil
CN113439834A (en) * 2020-03-25 2021-09-28 广东省禾基生物科技有限公司 Preparation method of water lily flower cell water and application of water lily flower cell water
CN112481035A (en) * 2020-11-18 2021-03-12 河北中烟工业有限责任公司 Extraction method of fresh lotus essential oil

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