CN104862079A - Method for extracting essential oil from trigonella foenum-graecum leaves - Google Patents
Method for extracting essential oil from trigonella foenum-graecum leaves Download PDFInfo
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- CN104862079A CN104862079A CN201510276490.2A CN201510276490A CN104862079A CN 104862079 A CN104862079 A CN 104862079A CN 201510276490 A CN201510276490 A CN 201510276490A CN 104862079 A CN104862079 A CN 104862079A
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- essential oil
- trigonella
- blade
- trigonella foenum
- graecum
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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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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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
- 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
- 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
- C11B9/027—Recovery of volatiles by distillation or stripping
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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)
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- Fats And Perfumes (AREA)
Abstract
The invention discloses a method for extracting essential oil from trigonella foenum-graecum leaves. The method comprises the following steps: firstly kneading the trigonella foenum-graecum leaves with hands until the juice is just squeezed out, naturally airing the trigonella foenum-graecum leaves, crushing and screening the leaves to obtain powder of the trigonella foenum-graecum leaves; secondly, mixing the leaf powder with absolute ethyl alcohol according to the mass ratio of 1:85 (g/ml), and preparing a mixture; then placing the mixture into a water bath kettle at the temperature of 55 DEG C, and performing water bath for 21 hours; centrifuging for 30 minutes according to the revolving speed of 5000 r/min, collecting the supernatant and filling the supernatant into a test tube; finally placing the test tube into the water bath kettle at the temperature of 85 DEG C, and heating for 4.2 hours, so as to obtain the remained part as the final extract which is the essential oil of trigonella foenum-graecum when ethanol is completely volatilized. According to the method for extracting the essential oil from the trigonella foenum-graecum leaves disclosed by the invention, the essential oil is extracted by the steps of water bath, centrifuging, heating and separation; the method is accessible in raw materials, simple to process, high in extraction efficiency and convenient to operate; the content of the organic solvent remained in the extracted essential oil is low.
Description
Technical field
The invention belongs to medicine, food and technical field of chemical industry, particularly relate to a kind of method extracting trigonella blade essential oil.
Background technology
Trigonella is the seed of leguminous plants frenugreek spp trigonella (Trigonellafoenun-graecuL.), trigonella has another name called Remote Lemongrass Herb (" Shengjing city leads to will "), vanilla, eel grass, bitter piece dish, fragrant clover etc., for pulse family annual herb plant, complete stool has fragrance, extract herb during fruit maturation, lay seed, dry, life is used or micro-stir-fry is used, and is conventional Chinese medicine.Main product is in provinces such as China Tibet, Anhui, Sichuan, Ningxia, Gansu.Mainly there is warming the kidney to invigorate YANG, hernia, the disturbance of lower legs due to pathogenic cold and dampness, the soreness of waist, the impotence etc. of suffering from a deficiency of the kidney effect are trembled with fear in dispelling cold and dehumidification, treatment, are famous traditional Chinese medicine ingredients.Therefore, necessary trigonella composition and extracting method to be studied, trigonella principle active component is volatile oil, volatile oil is also known as essential oil, volatile oil ingredient more complicated, is made up of, substantially based on terpene, aromatics, fatty compounds, nitrogenous sulphur compounds etc. tens kinds of even hundreds of compounds mostly, but wherein often there is component shared by certain several composition comparatively large, medicine, food and chemical industry have important use.The plants essential oil of pure natural has following functions: fragrant, after natural fragrance enters brain via olfactory nerve, anterior lobe of cerebrum can be stimulated to secrete interior coffee to eliminate and two kinds of hormone eliminated by brain coffee, make spirit present the state of the most comfortable, this is the best good recipe of guarding soul.And different essential oils can combine mutually, mix the fragrance oneself liked, the speciality of essential oil can not be destroyed, make the with better function of essential oil on the contrary.Essential oil essence can anti-communicable disease, to antibacterium, virus, mould, can anti-inflammation, anti-spasm, promote cell metabolism and cell regeneration function, make life finer.And some essential oil energy endocrine regulation organ, promote hormone secretion, allow the physiology of human body and psychological activity, obtain good development.At present, the aromatic essential oil of 95% is extracted by distillation method and obtains, but when hot steam is filled in container, can by the volatile oil composition of plant internal memory along with water vapour evaporates.Solvent extration, this extraction mode is relatively costly, and reason is its complex procedures, and the position such as flower, petal, bud of traditional solvent extration extraction plant, the product first after extraction is called " congealed fat " (Concrete).If extraction is the natural secretion thing of plant, as natural gum, resin or tree cream, then product is first called " resin " (Resinoid).After product " resin " or " congealed fat " detach with alcohol or alcohols again first, the subordinate phase end-products obtained, is just called absolute oil (Absolute).Finally, then with volatile straight alcohol, the grease in face cream is washed away the absolute oil obtaining exquisite costliness, the essential oil yield extracted is also fewer.
At present, trigonella effective constituent is being studied the extraction of its effective constituent and essential oil from trigonella cauline leaf of extracting from its seed with ether mostly, but it is only limitted to by ether extraction, and extraction effect is poor, big for environment pollution, can't completely for suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of method extracting trigonella blade essential oil, be intended to solve current trigonella effective constituent and adopt ether extraction, extraction effect is poor, problem big for environment pollution.
The present invention is achieved in that a kind of method extracting trigonella blade essential oil, and the method for described extraction trigonella blade essential oil comprises the following steps:
First rubbing the blade hand of trigonella to just going out juice, allowing cytoclasis, oxydase can react further with organic substance, generates more essential oil.Naturally dry, allow moisture evaporate completely, grinding and sieving, obtain trigonella leaf powder, object makes blade become broken little, can fully contact with ethanol;
Secondly leaf powder and dehydrated alcohol being mixed by quality 1:85g/ml loads in triangular flask, fully stirs and allows leaf powder immerse dehydrated alcohol completely, allow leaf powder fully contact with ethanol, make mixture, seal triangular flask, prevent ethanol from volatilizing with glass stick;
Again mixture is put into 55 DEG C of water-bath water-bath 21h, allow the organic substance in vegetable cell discharge completely at a certain temperature, dissolve in ethanol; Then centrifugal 30min under rotating speed is 5000r/min, removing impurity, collects supernatant liquor, loads test tube;
Finally test tube is put into 85 DEG C of water-baths and heat 4.2h, allow ethanol volatilize rapidly at a certain temperature, detect ethanol content with chromium sulphate simultaneously, treat that ethanol vapors away completely, collect remainder and be the highly purified trigonella essential oil of extraction end product-high quality.
The invention provides the method extracting trigonella blade essential oil, by smudge cells, accelerate the combination of organism and enzyme, essential oil yield is significantly improved; Heating and water-bath make cell break further, allow essential oil fully be dissolved in ethanol, centrifugation impurity, to be further purified essential oil; Heating and separating ethanol, ethanol is volatilized fast, and essential oil purity improves, and the advantage of present method is that material is easy to get, process is simple, extraction efficiency is high, and essential oil content reaches 14%, and remaining organic solvent content in the essential oil extracted is little, ethanol content only remains 0.036%, ethanol also can fully recycling, and method is simple, easy to operate.
Accompanying drawing explanation
Fig. 1 is the method flow diagram of the extraction trigonella blade essential oil that the embodiment of the present invention provides;
Fig. 2 is the methanol extract crest schematic diagram that the embodiment of the present invention provides;
Fig. 3 is the dehydrated alcohol extraction object wave peak schematic diagram that the embodiment of the present invention provides;
Fig. 4 is the water extract crest schematic diagram that the embodiment of the present invention provides;
Fig. 5 is the superposition crest schematic diagram of three kinds of solvent extractable matters that the embodiment of the present invention provides;
In figure: ("-" represent methanol extract "---" represent dehydrated alcohol extraction thing " ... " represent water extract);
Fig. 6 is that the solvent that provides of the embodiment of the present invention affects schematic diagram to the extraction of trigonella effective constituent;
Fig. 7 be the extraction of the material comparison trigonella effective constituent that the embodiment of the present invention provides affect schematic diagram;
Fig. 8 is that the temperature that provides of the embodiment of the present invention affects schematic diagram to the extraction of trigonella effective constituent;
Fig. 9 affects schematic diagram to the extraction of trigonella effective constituent time of providing of the embodiment of the present invention;
Figure 10 is that the different rotating speeds that provides of the embodiment of the present invention affects schematic diagram to trigonella blade essential oil purity;
Figure 11 is the contrast schematic diagram of essential oil amount in the process that provides of the embodiment of the present invention and untreated trigonella blade.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The present invention utilizes trigonella leaf, application dehydrated alcohol, and extracted by water-bath, centrifugal, heating and separating, material is easy to get, and process is simple, and extraction efficiency is high, and remaining organic solvent content in the essential oil extracted is little, and step is simple, easy to operate.
Below in conjunction with accompanying drawing 1, extracting method of the present invention is described in detail:
S101: first rubbing the blade hand of trigonella to just going out juice, naturally drying, grinding and sieving, obtains trigonella leaf powder;
S102: secondly leaf powder and dehydrated alcohol are mixed by quality 1:85g/ml and load in triangular flask, fully stir with glass stick and allow leaf powder immerse dehydrated alcohol completely, make mixture, seal triangular flask;
S103: again the triangular flask that mixture is housed is put into 55 DEG C of water-bath water-bath 21h; Then proceed in 50ml centrifuge tube, centrifugal 30min under rotating speed is 5000r/min, collect supernatant liquor, load test tube;
S104: finally test tube is put into 85 DEG C of water-baths and heat 4.2h, detects ethanol content in mixed solution simultaneously, treats that ethanol vapors away completely, and take out test tube, remainder is extraction end product-trigonella essential oil.
By following experiment, detailed explanation is done to effect of the present invention:
1, experiment material
Trigonella fruit also non-fully matured time pluck its leaf, part hand is rubbed to just going out juice, naturally dries, and a part does not process, seasoning, collect after for subsequent use.
2, reagent
Reagent: methyl alcohol, water-ethanol, distilled water.
3, experimental technique
Take 5g trigonella powder, with methyl alcohol, water-ethanol, distilled water extracting effective components.Study four single factor test factors (solvent, material ratio, temperature, time) impact on essential oil proposition amount, with one of them factor for variable, three factors are constant tests for other.And the index such as centrifugal rotational speed, distillation temperature is studied.
4 experimental results
4.1 different solvents are on the impact of essential oil proposition amount
Select different solvents (methyl alcohol, dehydrated alcohol, distilled water), according to material than 1:50, temperature 40 DEG C, the time, 5h tested, and method is the same, utilized UV-2450 ultraviolet-visible pectrophotometer to measure the crest value of the extracting solution of the three kinds of solvents obtained.Shown in the following 2-Fig. 5 of result; Can obtain three kinds of solvents at wavelength by Fig. 5 is that peak-peak has appearred in 670nm simultaneously.Therefore in single factor test factorial analysis afterwards, this wavelength is adopted.
4.2 single factor test are to the impact analysis of extracting
4.2.1 solvent is on the impact of the extraction of trigonella effective constituent
50 times are diluted to the extracting solution of three kinds of solvents above simultaneously, measures absorbance value at wavelength 670nm place.Result as shown in Figure 6, the absorbance value of the extracting solution of methyl alcohol is maximum as seen from Figure 6, illustrate that methyl alcohol is the best solvent of trigonella extracts active ingredients, but, methyl alcohol is poisonous, can to environment, and, between methyl alcohol and extraction using alcohol amount, difference is little, and therefore best Extraction solvent is ethanol.
4.2.2 the impact of the extraction of comparison trigonella effective constituent is expected
Solvent: ethanol, temperature: 40 DEG C, time: 5h, expect that than gradient be 1:40 ~ ~ ~ 1:100, every 5 units are a gradient, 13 concentration gradients are set, extracting method is the same, result as shown in Figure 7, as seen from Figure 7, when expecting that ratio is 1:85, absorbance value is maximum, illustrates that 1:85 is the best material ratio of trigonella extracts active ingredients.
4.2.3 temperature is on the impact of the extraction of trigonella effective constituent
Solvent: ethanol, material ratio: 1:85, the time: 5h, extracting method is the same, and as shown in Figure 8, as seen from Figure 8, when temperature is 55 DEG C, absorbance value is maximum for result, illustrates that 55 DEG C is the optimum temperature value of trigonella extracts active ingredients.
4.2.4 the time is on the impact of the extraction of trigonella effective constituent
Solvent: ethanol, material ratio: 1:85, temperature: 55 DEG C, extracting method is the same, result as shown in Figure 9:
As seen from Figure 9, when the time is 21h, absorbance value is maximum, illustrates that 21h is the Best Times of trigonella extracts active ingredients.
4.3 different centrifugal rotational speeds are on the impact of trigonella blade essential oil purity
Get five groups of filtrates with whizzer at 3000r/min, 4000r/min, 5000r/min, 6000r/min, 7000r/min centrifugal 30 minutes respectively, as shown in Figure 10, it is larger that different centrifugal rotational speed extracts impact to trigonella blade essential oil amount; Time between 3000r/min to 5000r/min, essential oil amount obviously reduces along with the raising of rotating speed, centrifugal rotational speed increases, go deimpurity effect better, rotating speed is greater than 5000r/min essential oil amount and tends towards stability, rotating speed is higher larger to machine infringement, and to sum up factor obtains best centrifugal rotational speed and should be 5000r/min.
4.4 distillation temperatures are on the impact of trigonella blade essential oil amount
Get five groups of filtrates with whizzer under 5000r/min, centrifugal 30 minutes, centrifugate is distilled respectively in the water-bath of 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C and carries oil, record the indexs such as the colour-change of the volume of the residue ethanol of each time period, solution viscosity and solution and last ethanol volatilization complete time used; Result is as shown in table 1:
Table 1: the mensuration of trigonella blade extraction of essential oil optimal temperature
As shown in Table 1, Extracting temperature is 70 DEG C, 75 DEG C, 80 DEG C time, although the final essential oil color and luster extracted is good, quality is good, the time used is oversize, is unfavorable for extracting essential oil; Extracting temperature is 85 DEG C time, and the essential oil color and luster of extraction is good, quality is good, and the time used is shorter simultaneously; Although the time is short when 90 DEG C, essential oil chromaticness is poor, of poor quality, so choose 85 DEG C for optimal temperature.
The extraction yield of essential oil in 4.5 process and untreated trigonella blade
Get the filtrate of five groups of 1g process blades and untreated cauline leaf sheet respectively, at the centrifugal 30min of 5000r/min, extracting centrifugal liquid extracts essential oil in the water-bath of 85 DEG C, oily after weigh up essential oil amount, according to extraction of essential oil rate=trigonella powder quality × 100% of oil mass/take, calculating process trigonella blade extraction of essential oil rate is 14.4%, obtains untreated trigonella blade extraction of essential oil rate 10.7%, result as shown in figure 11:
In sum so the present invention takes alcohol extraction and water-bath distillation method to extract the essential oil in trigonella leaf, adopt alcohol extraction method extraction process, in trigonella blade, essential oil yield is high, the whole experimentation time is shorter, and whole process temperature is lower, thus ensure that derived essential oil can not be active impaired because of extraction.
By the present invention explore centrifugal rotational speed be 5000r/min, the material that obtains of Extracting temperature 85 DEG C and pre-stage test is 1:85 than (trigonella leaf: dehydrated alcohol), water-bath extraction temperature is 55 DEG C, water bath time is 21h time, in trigonella leaf, the extraction effect of essential oil is best.And the essential oil amount explored in process trigonella blade is a little more than the essential oil in untreated trigonella blade.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. extract a method for trigonella blade essential oil, it is characterized in that, the method for described extraction trigonella blade essential oil comprises the following steps:
First the blade hand of trigonella being rubbed to just going out juice, naturally drying, grinding and sieving, obtain trigonella leaf powder;
Secondly leaf powder and dehydrated alcohol being mixed by quality 1:85g/ml loads in triangular flask, fully stirs and allows leaf powder immerse dehydrated alcohol completely, make mixture, seal triangular flask with glass stick;
Again the triangular flask that mixture is housed is put into 55 DEG C of water-bath water-bath 21h; Then proceed in 50ml centrifuge tube, centrifugal 30min under rotating speed is 5000r/min, collect supernatant liquor, load test tube;
Finally test tube is put into 85 DEG C of water-baths and heat 4.2h, detect ethanol content in mixed solution simultaneously, treat that ethanol vapors away completely, take out test tube, remainder is extraction end product-trigonella essential oil.
2. one kind uses the application of trigonella blade essential oil in medicine described in claim 1.
3. one kind uses the application of trigonella blade essential oil in food described in claim 1.
4. one kind uses the application of trigonella blade essential oil in chemical industry described in claim 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111888387A (en) * | 2020-08-24 | 2020-11-06 | 广州立达尔生物科技股份有限公司 | Fenugreek essential oil enteric microcapsule preparation and preparation method thereof |
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