CN203247246U - Device for collecting natural flowery essential oil - Google Patents
Device for collecting natural flowery essential oil Download PDFInfo
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- CN203247246U CN203247246U CN 201320223662 CN201320223662U CN203247246U CN 203247246 U CN203247246 U CN 203247246U CN 201320223662 CN201320223662 CN 201320223662 CN 201320223662 U CN201320223662 U CN 201320223662U CN 203247246 U CN203247246 U CN 203247246U
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Abstract
The utility model relates to a device for collecting natural flowery essential oil which comprises a humidification air generator, a sample collecting chamber and a volatile constituent condensation receiver. According to the utility model, the fragrance degree of the volatile essential oil obtained by adopting the device provided by the utility model is closer to natural floral fragrance; through the gas chromatography-mass spectroscopy, compared with the traditional methods such as the headspace collecting method, the obtained volatile material contains more constituents, and has an enlarged compound boiling range; the obtained concentrates of the volatile constituent are subjected to gas chromatography or gas-mass combined analysis, so that the composition of the natural flowery essential oil can be determined; besides, the device can be used for flowering plant physiology and heredity research based on essential oil composition analysis.
Description
Technical field
The utility model relates to a kind of natural floral note essential oil " humidifying air method " gathering device.
Background technology
When gathering flowering plant volatile matter (essential oil), guarantee to collect as far as possible the volatile matter of plant under the state of nature.Except the methods such as traditional wet distillation, solvent extraction, solid-phase microextraction and dynamic head-space method are used commonplacely in the research of volatile matter at present.These methods respectively have characteristics, and simplified summary is as follows:
Wet distillation, mainly by steam evaporator, straight cold finger and susceptor form.Wet distillation has the large characteristics of batch processing amount, but easily makes easy decomposition and readily oxidizable substance generation chemical reaction, generates the derivative that does not have in the natural essence.
Solvent extration, generally adopting normal hexane is extraction agent, decompression and solvent recovery after the extraction, enriched material is target product.This method low-boiling point material easily loses, and target product generally all contains the non-volatile substances such as pigment.
Solid-phase Microextraction is newer Sampling techniques, need not organic solvent, and cost consumption is low, and required sample size is few, simple to operation fast, centralized procurement sample, extraction, simmer down to one, can with gas chromatography-mass spectrum (GC-MS) coupling.Its profile and device are more similar to common sampler, and its key position is a segment length 1cm, the fused quartz fiber of diameter 110 μ m.Its outer wall scribbles one deck GC stationary liquid, and the material of liquid film and thickness are determining its selectivity, only needs during sampling this fiber head is released syringe needle one end, places sample or head space gas.Need only during desorption fiber head is drawn back in the syringe needle directly to gas chromatographic sample introduction.Very convenient saving time in this way.But for the lower composition of those content, may fail to reach the detection limit of instrument and can not be detected owing to collection capacity.
The dynamic head-space method is inserted in the high-pressure polyethylene bag with the sampling section of plant, seals tight end opening; Or the sampling section of plant put into a semi-enclosed container, and between the opening of plant and container, fill out cotton, cut off extraneous air as far as possible.Pneumatic pump is sent into air in the sampler chamber behind active carbon filtration, the outlet of sampler chamber is connected with adsorption tube, and the volatile gases of absorptive collection plant, adsorption tube link to each other with pneumatic pump by gas circuit again, makes like this air cycle flow acquisitions adsorption sample.General make sorbent material with 2,6-phenylbenzene p-phenylene (Tenax TA) or the graphite mixture that contains 30%Tenax TA, the adsorption tube after the collection can pass through the thermal desorption device, and directly volatile matter importing GC or the GC-MS with collection measures.This sorbent material has good absorption property to lower boiling to the compound of higher, but for high boiling compound (more than 350 ℃), during thermal desorption, and quantitative desorption or have dead absorption.Also there is the possibility of decomposing in some heat-labile compounds when thermal desorption simultaneously.
The natural floral note essential oil humidifying air gathering device that the utility model relates to is the transformation of carrying out on the basis of head space acquisition method device.We are not difficult to find in daily life, behind the rain fragrance of a flower of flowering plant when fine more strong, illustrate that malaria can carry more fragrance of a flower material.Adopt the utility model device, utilize exactly the air of humidification as carrier, not only can simulate the physical environment with certain humidity, and can make the fresh growth conditions of the long-term maintenance of plant, thereby the volatile matter that collects can be more, and fragrance also should be closer to nature.This gathering device is made of concentrated receptor three parts of humidifying air producer, sample chamber and volatile component condensation.Substitute adsorption unit in the dynamic head-space method by the multi-stage condensing device, avoided the possibility of dead absorption or thermolability compound decomposition.Volatile essential oil to this method acquisition, carried out the GC-MS analysis, and be analyzed with same source essential oil that solvent extration and dynamic head-space method obtain, found that the volatile matter that the method obtains contains more composition, fragrance is more near nature, and the compound boiling range increases.
The utility model content
The purpose of this utility model is to provide a kind of effect to gather preferably the device of natural floral note essential oil.
A kind of natural floral note essential oil gathering device, comprise the humidifying air producer of connecting by pipeline successively, sample collecting chamber and volatile component condensation receptor, described humidifying air producer comprises the container body for water storage, described water container is provided with the gas inlet, water inlet and humidifying air outlet, the external compression source of the gas stretches to the bottom of water container by pipeline connection gas inlet and pipeline, the humidifying air outlet connects the sample collecting chamber, the airtight Glass Containers of the plant that blooms is deposited for being used in described sample collecting chamber, and described volatile component condensation receptor comprises prolong, receiving vessel and cold-trap; The prolong tail end connects receiving vessel, and receiving vessel places cold-trap; Described prolong front end connects the sample collecting chamber by pipeline.
Refrigerant in the described prolong is circulating cooling liquid.
The quantity of described volatile component condensation receptor is at least one; When surpassing one, prolong is connected in series.
Utilize the method for described natural floral note essential oil gathering device collection essential oil,
(1) with air through activated carbon filtration, pass in the humidifying air producer that water is housed through the gas inlet, air emerged from the bottom of water and form damp atmosphere with water molecules;
(2) the potted plant plant that blooms is enclosed in the sample collecting chamber;
(3) prolong adopts the aqueous solution circulating condensing of ethylene glycol, and the mixture of putting into dry ice and ethanol in the cold-trap gathers.
Described air is the pressurized air 0.05～0.20MPa that reduces pressure.Optimum is 0.1MPa, makes existing air flowing in the system, and is again can not pressure excessive, guarantees to bloom plant near outdoor state of nature.
The aqueous solution mass concentration of ethylene glycol is 20%～80%; Can keep-18 ℃～-35 ℃ low temperature, optimum is 50%, at this moment can keep-30 ℃ low temperature, and it is too high that soltion viscosity also is unlikely to; Receiving bottle should immerse in dry ice/ethanol fully, can keep-40 ℃～-60 ℃ low temperature.
The proportioning of dry ice/ethanol is 1:2～1:1(volume ratio), dry ice/ethanol container can add asbestos heat-insulating sleeve; Volatile component is held back in abundant condensation such as need, can be connected in series many group condensation receptors.
The volatile essential oil that obtains and the mixture of water, through leaving standstill of certain hour, the profit natural layering, namely separable with separating funnel; If the amount of gained volatile oil is very few, can adopt a small amount of non-polar organic solvent (normal hexane) that oil-water mixture is extracted, keep organic phase, be used for after the drying analyzing and measure.
The utility model makes the fresh growth conditions of the long-term maintenance of flowers by the physical environment of the certain humidity of simulation, gathers the extrait oil mass that obtains more, and fragrance is also closer to the natural fragrance of a flower.Analyze discovery by GC-MS, this method is compared with solvent extration and dynamic head-space method, and contained volatile constituent is more in the essential oil, and each composition collocation is comparatively even, and the compound boiling range increases.
Description of drawings
Fig. 1 is the utility model setting drawing;
Wherein 1 is the humidifying air producer, and 2 is the sample collecting chamber, and 3 is volatile component condensation receptor, and 4 is the container body of water storage, and 5 is the gas inlet, and 6 is water inlet, and 7 are the humidifying air outlet, and 8 is prolong, and 9 is receiving vessel, and 10 is cold-trap.
Embodiment
Following examples are to further specify of the present utility model, are not to restriction of the present utility model.
Embodiment 1:
The utility model natural floral note essential oil gathering device, comprise the humidifying air producer 1 of connecting by pipeline successively, sample collecting chamber 2 and volatile component condensation receptor 3, described humidifying air producer 1 comprises the container body 4 for water storage, described water container 4 is provided with gas inlet 5, water inlet 6 and humidifying air outlet 7, the external compression source of the gas stretches to the bottom of water container 4 by pipeline connection gas inlet 5 and pipeline, humidifying air outlet 7 connects sample collecting chamber 2, the airtight Glass Containers of the plant that blooms is deposited for being used in described sample collecting chamber 2, and described volatile component condensation receptor 3 comprises prolong 8, receiving vessel 9 and cold-trap 10; Prolong 8 one ends connect receiving vessel 9, and receiving vessel 9 places cold-trap 10; Described prolong 8 the other ends connect sample collecting chamber 2 by pipeline.
Using the utility model device to carry out the natural floral note essential oil gathers with the composition analysis step as follows:
1) preparation of samples: use is device as shown in drawings, prepares a basin just at rose in full bloom (band soil), adopts cotton, plasticine and adhesive tape etc. to seal the stem stalk of rose and the space of container bottom tight;
2) gather: open the aqueous glycol solution circulation device, the circulation fluid upper temperature limit is set is-30 ℃, be limited to-35 ℃ down; When the circulation fluid temperature reaches-30 ℃, add dry ice and ethanol to collector, ethanol just submergence dry ice is advisable; Open compression steel cylinder main valve, regulating reducing valve is 0.1MPa to air pressure, gathers beginning, moves continuously 48 hours, can obtain the mixture of a certain amount of volatile essential oil and water, and profit layering behind the sufficient standing can separate by separating funnel; If the amount of volatile oil is very few, can adopt a small amount of non-polar organic solvent (normal hexane) that oil-water mixture is extracted, keep organic phase, be used for after the drying analyzing and measure;
3) GC measures: no matter be volatile oil or volatile oil hexane solution, carry out drying with anhydrous sodium sulphate before analyzing mensuration; The purpose of carrying out the GC analysis is to be the best chromatographic separation condition of GC-MS Analysis deterrmination: Agilent 7890 type gas chromatographs; Sampling volume 2 μ L; Sampler temperature (250 ℃); Chromatographic column type (HP-5 capillary column, 60m * 0.25mm i.d., thickness of liquid film 0.25 μ m); Carrier gas is helium (purity＞99.995%), flow velocity 1mL/min; Column temperature is temperature programming (initial 50 ℃, keep 10min, then the speed with 5 ℃/min rises to 230 ℃); Signal detector is flame ionization detector;
4) GC-MS measures: by best GC condition sample introduction, carry out the full scan pattern and measure, obtain a series of mass-spectrometric datas, carry the mass spectrum picture library with instrument and compare, and determine each component relative mass mark by area normalization, finish the composition of each chromatographic peak and differentiate and assay.
Embodiment 2:
2 kinds of Flos Rosae Rugosae quintessence oil compositions comparative analysis that the Flos Rosae Rugosae quintessence oil that obtains among the embodiment 1 and solvent extration and head space acquisition method obtain, find that the volatile oil that the utility model device obtains contains 29 kinds of compositions, the solvent extration essential oil contains 20 kinds of compositions, dynamic head-space method essential oil contains 26 kinds of compositions, the results are shown in Table 1.
Identical with the head space acquisition method with solvent extration is, the rhodamine b extra 500 main body of oil of humidifying air method collection is β-geraniol, β-vernol, α-Geraniol and geraniol acetate, and wherein geraniol, Geraniol and ester class thereof are the main components that determines rose scent; Different is that the Flos Rosae Rugosae quintessence oil of humidifying air method collection contains more Eugenol, farnesol and various alkane.Eugenol is hot fragrant composition, and mainly auxiliary rose is fragrant and sweet, makes fragrance sweet dense, and farnesol can make fragrance strong, and is complementary with delicate fragrance composition rose oxide, and straight-chain paraffin can play the fixation effect, makes fragrance lasting.On the whole, the Flos Rosae Rugosae quintessence oil that collects owing to the humidifying air method contains than multicomponent, and each composition collocation evenly, thereby makes fragrance plump full, and fragrance is lasting, and the essential oil grade is higher.
The Flos Rosae Rugosae quintessence oil composition analysis result that three kinds of different methods of table 1 gather
Claims (3)
1. natural floral note essential oil gathering device, it is characterized in that, comprise the humidifying air producer of connecting by pipeline successively, sample collecting chamber and volatile component condensation receptor, described humidifying air producer comprises the container body for water storage, described water container is provided with the gas inlet, water inlet and humidifying air outlet, the external compression source of the gas stretches to the bottom of water container by pipeline connection gas inlet and pipeline, the humidifying air outlet connects the sample collecting chamber, the airtight Glass Containers of the plant that blooms is deposited for being used in described sample collecting chamber, and described volatile component condensation receptor comprises prolong, receiving vessel and cold-trap; The prolong tail end connects receiving vessel, and receiving vessel places cold-trap; Described prolong front end connects the sample collecting chamber by pipeline.
2. a kind of natural floral note essential oil gathering device according to claim 1 is characterized in that, the refrigerant in the described prolong is circulating cooling liquid.
3. a kind of natural floral note essential oil gathering device according to claim 1 is characterized in that, the quantity of described volatile component condensation receptor is at least one; When surpassing one, prolong is connected in series.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320223662 CN203247246U (en) | 2013-04-27 | 2013-04-27 | Device for collecting natural flowery essential oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201320223662 CN203247246U (en) | 2013-04-27 | 2013-04-27 | Device for collecting natural flowery essential oil |
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| CN203247246U true CN203247246U (en) | 2013-10-23 |
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| CN 201320223662 Expired - Fee Related CN203247246U (en) | 2013-04-27 | 2013-04-27 | Device for collecting natural flowery essential oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371828A (en) * | 2014-11-14 | 2015-02-25 | 雷宏师 | Equipment for extracting jasmine flower perfume essence and essential oil by adopting air current circulation method |
| CN110672386A (en) * | 2018-07-02 | 2020-01-10 | 长谷川香料株式会社 | Fragrance collection system, fragrance collection method, fragrance liquid, fragrance composition, and blended fragrance |
-
2013
- 2013-04-27 CN CN 201320223662 patent/CN203247246U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371828A (en) * | 2014-11-14 | 2015-02-25 | 雷宏师 | Equipment for extracting jasmine flower perfume essence and essential oil by adopting air current circulation method |
| CN104371828B (en) * | 2014-11-14 | 2017-04-05 | 雷宏师 | Circulation of air flow method extracts the equipment of jasmine flower perfume and quintessence oil |
| CN110672386A (en) * | 2018-07-02 | 2020-01-10 | 长谷川香料株式会社 | Fragrance collection system, fragrance collection method, fragrance liquid, fragrance composition, and blended fragrance |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131023 Termination date: 20140427 |