CN106701321A - Piper magen essential oil and extraction and chemical component analysis method thereof - Google Patents
Piper magen essential oil and extraction and chemical component analysis method thereof Download PDFInfo
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- CN106701321A CN106701321A CN201710059926.1A CN201710059926A CN106701321A CN 106701321 A CN106701321 A CN 106701321A CN 201710059926 A CN201710059926 A CN 201710059926A CN 106701321 A CN106701321 A CN 106701321A
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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
- C11B9/022—Refining
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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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8813—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials
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Abstract
The invention provides piper magen essential oil, an extraction method of the essential oil, and a method for analyzing chemical components of the essential oil. The extraction method comprises the following steps: by taking stems of piper magen as raw materials, extracting essential oil by using a steam distillation method, wherein the distillation temperature is 95-120 DEG C and the distillation time is 0.5-8 hours; and performing oil-water separation on the distilled liquid, and drying the oil part by using anhydrous sodium sulfate, thereby obtaining the piper magen essential oil. The essential oil extracted from the piper magen stems is unique and scented in aroma. The invention further provides a method for analyzing the chemical components of the piper magen essential oil. 28 chemical components are identified from the piper magen essential oil by utilizing gas chromatography-mass spectrography (GC-MS). The piper magen essential oil technology provided by the invention can provide quality control standards for applications of the piper magen essential oil in preparation of cosmetics, food additives, tobacco essence, essence for washing products and medicinal essence.
Description
Technical field：
The invention belongs to natural product extraction separation technology field, more particularly to snippings essential oil is prepared and its chemical composition
Analysis method.
Background technology：
Snippings (Piper magen) is Piperaceae pepper platymiscium, is the edible one kind of In Xishuangbanna of Yunnan ethnic group
Spice berry [a. journeys must Xishuangbanna ethnic group by force flavorant plant fragrance flavor and cosmetics, 1991, (3), 27-
31；B. journey must be strong, and thrifty Subtropical Regions of Yunnan spice berry Kunming is learned in analogy:Publishing house of Yunnan University .1995；C. Li Yan brightness,
Pei Shengji, perhaps Higher Plant Catalogue Kunming, richness Xishuangbanna again:Yunnan's Ethnic publishing house .1996].But its flavor component and its
Its chemical composition is unclear always.Snippings essential oil is extracted, and analyzes the main chemical compositions understood in essential oil, to snippings
And its exploitation of essential oil, it is significant.
The content of the invention：
The present invention is in view of the above-mentioned problems existing in the prior art, there is provided the preparation method of snippings essential oil, and snippings essential oil
The analysis method of chemical composition.
In order to realize above-mentioned purpose of the invention, the invention provides following technical scheme：
Snippings method of extraction of essential oil, the method extracts essential oil, distillation with the stem of snippings as raw material using steam distillation
Temperature is 95-120 DEG C, and distillation time is 0.5-8 hours, the liquid for distilling out, by water-oil separating, oily part anhydrous slufuric acid
Sodium is dried, and obtains snippings essential oil.
According to described snippings method of extraction of essential oil, be transferred to snippings stem drying and crushing in round-bottomed flask by the method, to
Added water in round-bottomed flask, shaken up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask, heated in round-bottomed flask with electric jacket
Water keeps micro-boiling, vapor air-distillation 6 hours, the liquid anhydrous sodium sulfate drying for distilling out to obtain water white transparency to seething with excitement
Liquid snippings essential oil.
Snippings Essential Oil method, the method stem first with snippings is carried as raw material using steam distillation
Essential oil is taken, vapo(u)rizing temperature is 95-120 DEG C, and distillation time is 0.5-8 hours, the liquid for distilling out, by water-oil separating, oily portion
Divide and use anhydrous sodium sulfate drying, obtain snippings essential oil；Or first snippings stem drying and crushing is transferred in round-bottomed flask, burnt to round bottom
Added water in bottle, shaken up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask, heating water in round-bottomed flask with electric jacket extremely boils
Rise, keep micro-boiling, vapor air-distillation 6h, the liquid anhydrous sodium sulfate drying for distilling out to obtain colourless transparent liquid snippings
Essential oil；Then chemical composition and content contained by gas chromatography-mass spectrum GC-MS condition analysis snippings essential oils are further used.
Method, snippings essential oil gas chromatography-mass spectrum GC-MS condition analysis are analysed according to described snippings Chemical Composition of The Essential Oil
Its contained chemical composition and content are：Nonane 0.122%, australene 0.095%, down alkene 0.040%, sabinene 0.050%, β-
Firpene 0.139%, limonene 0.047%, γ-terpinene 0.050%, linalool 1.426%, pine tar -4- alcohol 0.349%, α -
Terpinol 0.088%, capraldehyde 27.512%, decyl alcohol 42.964%, Bronyl acetate 1.120%, tridecane 0.468, capric acid
3.251%, α-pepper alkene 0.117%, β-orange green pepper alkene 0.059, dodecanal 6.425%, β-carypohyllene 1.338%, α-China pink
Alkene 0.105%, dodecanol 5.757%, pentadecane 0.298%, δ-cadinene 0.100%, nerolidol 0.777%, bay
Acid 0.823%, caryophyllene oxide 0.507, myristic aldehyde 0.760%, pellitorine 0.980%.
According to described snippings Essential Oil method, the gas chromatography-mass spectrum GC-MS condition analysis instruments
It is Agilent Technologies companies of U.S. HP6890GC/5973MS gas chromatograph-mass spectrometer (GC-MS)s, GC conditions are：HP‐
5MS quartz capillary columns 30mm × 0.25mm × 0.25 μm；Column temperature：80 DEG C of initial temperature, 3 DEG C/min to 280 DEG C of temperature programming,
Keep 30min；Column flow is 1.0mL/min；250 DEG C of injector temperature；100kPa is pressed before post；The μ L of sample size 0.4；Split ratio
20:1；Carrier gas is high-purity helium, MS conditions：Ionization mode EI；Electron energy 70；250 DEG C of transmission line temperature；Ion source temperature
230℃；150 DEG C of quadrupole rod temperature；Mass range 35~500；It is qualitative using wiley7n.l standard library searchings.
Snippings essential oil, is obtained by following methods：Stem with snippings extracts essential oil as raw material using steam distillation, steams
It is 95-120 DEG C to evaporate temperature, and distillation time is 0.5-8 hours, the liquid for distilling out, and by water-oil separating, anhydrous sulphur is used in oil part
Sour sodium is dried, and obtains snippings essential oil.
Snippings essential oil, is obtained by following methods：The stem drying and crushing of snippings is transferred in round-bottomed flask, is burnt to round bottom
Added water in bottle, shaken up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask, heating water in round-bottomed flask with electric jacket extremely boils
Rise, keep micro-boiling, vapor air-distillation 6 hours, the liquid anhydrous sodium sulfate drying for distilling out to obtain colourless transparent liquid fiber crops
Root essential oil.
Chemical composition and content are contained by the snippings essential oil：Nonane 0.122%, australene 0.095%, down alkene
0.040%, sabinene 0.050%, nopinene 0.139%, limonene 0.047%, γ-terpinene 0.050%, linalool
1.426%, pine tar -4- alcohol 0.349%, alpha-terpineol 0.088%, capraldehyde 27.512%, decyl alcohol 42.964%, Bronyl acetate
1.120%, tridecane 0.468, capric acid 3.251%, α-pepper alkene 0.117%, β-orange green pepper alkene 0.059, dodecanal
6.425%, β-carypohyllene 1.338%, α-carypohyllene 0.105%, dodecanol 5.757%, pentadecane 0.298%, δ-needle juniper
Alkene 0.100%, nerolidol 0.777%, laurate 0.823%, caryophyllene oxide 0.507, myristic aldehyde 0.760%, wall
Potash 0.980%.
Snippings essential oil, it is prepared by following methods：Snippings stem drying and crushing, weighs the snippings sample 200 after crushing
Gram, it is transferred in 2 liters of round-bottomed flask, to being added water in round-bottomed flask 1.5 liters, shake up, glass extraction of essential oil is put on round-bottomed flask
Device and condenser pipe, heat water in round-bottomed flask and, to seething with excitement, keep micro-boiling with electric jacket, and vapor air-distillation 6 hours is distilled out
Liquid anhydrous sodium sulfate drying, colourless transparent liquid snippings essential oil is obtained, then using gas chromatography-mass spectrum GC-MS bars
Part, analyzing chemical composition and content contained by above-mentioned snippings essential oil is：Nonane 0.122%, australene 0.095%, down alkene
0.040%, sabinene 0.050%, nopinene 0.139%, limonene 0.047%, γ-terpinene 0.050%, linalool
1.426%, pine tar -4- alcohol 0.349%, alpha-terpineol 0.088%, capraldehyde 27.512%, decyl alcohol 42.964%, Bronyl acetate
1.120%, tridecane 0.468, capric acid 3.251%, α-pepper alkene 0.117%, β-orange green pepper alkene 0.059, dodecanal
6.425%, β-carypohyllene 1.338%, α-carypohyllene 0.105%, dodecanol 5.757%, pentadecane 0.298%, δ-needle juniper
Alkene 0.100%, nerolidol 0.777%, laurate 0.823%, caryophyllene oxide 0.507, myristic aldehyde 0.760%, wall
Potash 0.980%.
Described snippings essential oil is as quality control standard in allotment cosmetics, food additives, tobacco essence, washing
Application in product essence and medicinal essence.
The present invention has filled up the blank in terms of snippings essential oil research, and the technology that the present invention is provided can adjusted for snippings essential oil
Quality control standard is provided with cosmetics, food additives, tobacco essence, washing product essence and medicinal essence aspect.
Specific embodiment：
Essentiality content of the invention is further illustrated with embodiments of the invention below, but this is not limited with this
Invention.
Embodiment 1：
Snippings method of extraction of essential oil.Snippings stem drying and crushing, weighs 200 grams of snippings sample after crushing, and is transferred to 2 liters
In round-bottomed flask, to being added water in round-bottomed flask 1.5 liters, shake up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask.Electricity consumption
Water keeps micro-boiling, vapor air-distillation 6 hours to seething with excitement in hot jacket heating round-bottomed flask.The anhydrous sulphur of the liquid for distilling out
Sour sodium is dried, and obtains 0.257 gram of colourless transparent liquid, as snippings essential oil, and recovery rate is 0.13%.The gas that the essential oil gives out
Taste is unique and pure and fresh.
Embodiment 2：
Snippings method of extraction of essential oil.Snippings stem drying and crushing, weighs 200 grams of snippings sample after crushing, and is transferred to 2 liters
In round-bottomed flask, to being added water in round-bottomed flask 1.5 liters, shake up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask.Electricity consumption
Water keeps micro-boiling, vapor air-distillation 4 hours to seething with excitement in hot jacket heating round-bottomed flask.The anhydrous sulphur of the liquid for distilling out
Sour sodium is dried, and obtains 0.135 gram of colourless transparent liquid, as snippings essential oil, and recovery rate is 0.068%.
Embodiment 3：
Snippings method of extraction of essential oil.Snippings stem drying and crushing, weighs 200 grams of snippings sample after crushing, and is transferred to 2 liters
In round-bottomed flask, to being added water in round-bottomed flask 1.5 liters, shake up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask.Electricity consumption
Water keeps micro-boiling, vapor air-distillation 8 hours to seething with excitement in hot jacket heating round-bottomed flask.The anhydrous sulphur of the liquid for distilling out
Sour sodium is dried, and obtains 0.262 gram of colourless transparent liquid, as snippings essential oil, and recovery rate is 0.13%.The gas that the essential oil gives out
Taste is unique and pure and fresh.
Embodiment 4：
The chemical composition of the snippings essential oil that analysis embodiment 1 is obtained：Using gas chromatography-mass spectrum (GC-MS) condition.Instrument
It is Agilent Technologies companies of U.S. HP6890GC/5973MS gas chromatograph-mass spectrometer (GC-MS)s.GC conditions：HP‐
5MS quartz capillary columns (30mm × 0.25mm × 0.25 μm)；Column temperature：80 DEG C of initial temperature, temperature programming 3 DEG C/min to 280
DEG C, keep 30min；Column flow is 1.0mL/min；250 DEG C of injector temperature；100kPa is pressed before post；The μ L of sample size 0.4；Shunting
Than 20:1；Carrier gas is high-purity helium.MS conditions：Ionization mode EI；Electron energy 70；250 DEG C of transmission line temperature；Ion source temperature
230℃；150 DEG C of quadrupole rod temperature；Mass range 35~500；It is qualitative using wiley7n.l standard library searchings.
What snippings essential oil GC-MS was analyzed the results are shown in Table 1.
Table 1. snippings essential oil gas chromatography-mass spectrum (GC-MS) combination analysis result
Embodiment 5
The drop of snippings essential oil 1~2 (about 0.05~0.1 milliliter) is taken, is added in 100 grams of dry condiment, can be used for making
Dip in water, or barbecue condiment.
Claims (10)
1. snippings method of extraction of essential oil, it is characterised in that the method is extracted with the stem of snippings as raw material using steam distillation
Essential oil, vapo(u)rizing temperature is 95-120 DEG C, and distillation time is 0.5-8 hours, the liquid for distilling out, by water-oil separating, oily part
With anhydrous sodium sulfate drying, snippings essential oil is obtained.
2. snippings method of extraction of essential oil according to claim 1, it is characterised in that the method turns snippings stem drying and crushing
Move in round-bottomed flask, to being added water in round-bottomed flask, shake up, glass extraction of essential oil device and condenser pipe, electricity consumption are put on round-bottomed flask
Water keeps micro-boiling, vapor air-distillation 6h, the liquid anhydrous sodium sulfate for distilling out to seething with excitement in hot jacket heating round-bottomed flask
Dry, obtain colourless transparent liquid snippings essential oil.
3. snippings Essential Oil method, it is characterised in that the method stem first with snippings as raw material, using water vapour
The way of distillation extracts essential oil, and vapo(u)rizing temperature is 95-120 DEG C, and distillation time is 0.5-8 hours, the liquid for distilling out, by profit point
From oily part anhydrous sodium sulfate drying obtains snippings essential oil；Or first snippings stem drying and crushing is transferred in round-bottomed flask, to
Added water in round-bottomed flask, shaken up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask, heated in round-bottomed flask with electric jacket
Water keeps micro-boiling, vapor air-distillation 6 hours, the liquid anhydrous sodium sulfate drying for distilling out to obtain water white transparency to seething with excitement
Liquid snippings essential oil；Then further using chemical composition contained by gas chromatography-mass spectrum GC-MS condition analysis snippings essential oils and contain
Amount.
4. snippings Chemical Composition of The Essential Oil according to claim 3 analyses method, it is characterised in that and snippings essential oil gas-chromatography-
Its contained chemical composition of mass spectrum GC-MS condition analysis and content are：Nonane 0.122%, australene 0.095%, down alkene
0.040%, sabinene 0.050%, nopinene 0.139%, limonene 0.047%, γ-terpinene 0.050%, linalool
1.426%, pine tar -4- alcohol 0.349%, alpha-terpineol 0.088%, capraldehyde 27.512%, decyl alcohol 42.964%, Bronyl acetate
1.120%, tridecane 0.468, capric acid 3.251%, α-pepper alkene 0.117%, β-orange green pepper alkene 0.059, dodecanal
6.425%, β-carypohyllene 1.338%, α-carypohyllene 0.105%, dodecanol 5.757%, pentadecane 0.298%, δ-needle juniper
Alkene 0.100%, nerolidol 0.777%, laurate 0.823%, caryophyllene oxide 0.507, myristic aldehyde 0.760%, wall
Potash 0.980%.
5. snippings Essential Oil method according to claim 3, it is characterised in that：Gas-chromatography-the matter
Spectrum GC-MS condition analysis instrument is Agilent Technologies companies of U.S. HP6890GC/5973MS gas chromatography-mass spectrums
Combined instrument, GC conditions are：HP-5MS quartz capillary columns 30mm × 0.25mm × 0.25 μm；Column temperature：80 DEG C of initial temperature, program
Heat up 3 DEG C/min to 280 DEG C, keep 30min；Column flow is 1.0mL/min；250 DEG C of injector temperature；100kPa is pressed before post；
The μ L of sample size 0.4；Split ratio 20:1；Carrier gas is high-purity helium, MS conditions：Ionization mode EI；Electron energy 70；Transmission line temperature
250℃；230 DEG C of ion source temperature；150 DEG C of quadrupole rod temperature；Mass range 35~500；Examined using wiley7n.l standard spectrums storehouse
Rope is qualitative.
6. snippings essential oil, it is characterised in that the snippings essential oil is obtained by following methods：Stem with snippings is steamed as raw material using water
Steam distillation method extracts essential oil, and vapo(u)rizing temperature is 95-120 DEG C, and distillation time is 0.5-8 hours, the liquid for distilling out, by profit
Separate, oily part anhydrous sodium sulfate drying obtains snippings essential oil.
7. snippings essential oil, it is characterised in that the snippings essential oil is obtained by following methods：By the stem drying and crushing of snippings, it is transferred to
In round-bottomed flask, to being added water in round-bottomed flask, shake up, glass extraction of essential oil device and condenser pipe are put on round-bottomed flask, use electric jacket
Water keeps micro-boiling to seething with excitement in heating round-bottomed flask, and vapor air-distillation 6h, the liquid for distilling out is dry with anhydrous sodium sulfate
It is dry, obtain colourless transparent liquid snippings essential oil.
8. the snippings essential oil according to claim 6 or 7, it is characterised in that chemical composition and content contained by the snippings essential oil
For：Nonane 0.122%, australene 0.095%, down alkene 0.040%, sabinene 0.050%, nopinene 0.139%, limonene
0.047%, γ-terpinene 0.050%, linalool 1.426%, pine tar -4- alcohol 0.349%, alpha-terpineol 0.088%, capraldehyde
27.512%, decyl alcohol 42.964%, Bronyl acetate 1.120%, tridecane 0.468, capric acid 3.251%, α-pepper alkene
0.117%, β-orange green pepper alkene 0.059, dodecanal 6.425%, β-carypohyllene 1.338%, α-carypohyllene 0.105%, dodecane
Alcohol 5.757%, pentadecane 0.298%, δ-cadinene 0.100%, nerolidol 0.777%, laurate 0.823%, carypohyllene
Oxide 0.507, myristic aldehyde 0.760%, pellitorine 0.980%.
9. snippings essential oil, it is characterised in that it is prepared by following methods：Snippings stem drying and crushing, weighs the snippings after crushing
200 grams of sample, is transferred in 2 liters of round-bottomed flask, to being added water in round-bottomed flask 1.5 liters, shakes up, and glass essence is put on round-bottomed flask
Oil extractor and condenser pipe, heat water in round-bottomed flask and extremely seethe with excitement with electric jacket, holding micro-boiling, vapor air-distillation 6 hours,
The liquid anhydrous sodium sulfate drying for distilling out, obtains colourless transparent liquid snippings essential oil, then using gas chromatography-mass spectrum
GC-MS conditions, analyzing chemical composition and content contained by above-mentioned snippings essential oil is：Nonane 0.122%, australene 0.095%, down alkene
0.040%, sabinene 0.050%, nopinene 0.139%, limonene 0.047%, γ-terpinene 0.050%, linalool
1.426%, pine tar -4- alcohol 0.349%, alpha-terpineol 0.088%, capraldehyde 27.512%, decyl alcohol 42.964%, Bronyl acetate
1.120%, tridecane 0.468, capric acid 3.251%, α-pepper alkene 0.117%, β-orange green pepper alkene 0.059, dodecanal
6.425%, β-carypohyllene 1.338%, α-carypohyllene 0.105%, dodecanol 5.757%, pentadecane 0.298%, δ-needle juniper
Alkene 0.100%, nerolidol 0.777%, laurate 0.823%, caryophyllene oxide 0.507, myristic aldehyde 0.760%, wall
Potash 0.980%.
10. the snippings essential oil described in claim 6 or 7 or 9 as quality control standard allotment cosmetics, food additives,
Application in tobacco essence, washing product essence and medicinal essence.
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