CN103235061A - Pretreatment method for essence gas chromatography-mass spectrometry combination detection - Google Patents
Pretreatment method for essence gas chromatography-mass spectrometry combination detection Download PDFInfo
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- CN103235061A CN103235061A CN 201310104973 CN201310104973A CN103235061A CN 103235061 A CN103235061 A CN 103235061A CN 201310104973 CN201310104973 CN 201310104973 CN 201310104973 A CN201310104973 A CN 201310104973A CN 103235061 A CN103235061 A CN 103235061A
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Abstract
The invention relates to a pretreatment method for essence gas chromatography-mass spectrometry combination detection. The pretreatment method comprises the following steps: taking an essence sample, placing the sample into a 50 mL centrifuge tube, uniformly mixing carbon tetrachloride and acetone to obtain a mixing solution, sucking the mixing solution, injecting from the bottom of the centrifuge tube to form a uniform emulsion, carrying out ultrasound on an ultrasonic cleaning device, placing on a vortex mixer to shock, taking, carrying out centrifugation, removing the lower layer supernatant, carrying out blow-drying, adding acetone, carrying out volume metering to achieve a volume of 1 mL, and adding to an instrumental to analyze. The pretreatment method has characteristics of simpleness, easy operation, short time and good effect.
Description
Technical field
The present invention relates to the pre-treating method that a kind of essence detects, be specifically related to a kind of ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method for the detection of essence gas chromatography combined with mass spectrometry.
Background technology
Pre-treating method commonly used at present mainly contains following several: the solid-phase microextraction partition method is the sample pre-separation enrichment method that grows up the nineties in 20th century, it integrates sample pretreatment and sample introduction, will can combine with various analytical approachs after sample purifying, the enrichment and be specially adapted to organic assay determination.But also there is certain deficiency in SPME, a little less than the fused quartz fiber is highly brittle, is easy to fracture, and operation is very careful.The fiber stationary phase volume is little, and it is very limited to be adsorbed phase fragrance absolute mass, and the detection limit of fragrance is low, exigent production precision simultaneously, and any lack of standardization and inhomogeneity all can have influence on the surface nature of coating and the repeatability of extracting operation.The distillation extraction method is a kind of method of extracting volatile ingredient that Nickeron and Likens come out development in 1966 simultaneously, and this device collection extracts, distills, extracts, concentrates in one, has reduced operation steps, and is simple to operate, the extraction efficiency height; Simultaneously significant disadvantages is that the artifact that produces of long-time thermophilic digestion is more, and the analytic liquid that obtains has tangible fragrance distortion phenomenon.Liquid-liquid extraction belongs to classical solvent extraction and separation technology, and it is that a kind of component to be measured and sample matrices dissolubility difference in immiscible two-phase of utilizing purifies the method for extraction, but easily loses at operating process fragrance.Solid-Phase Extraction is a kind of adsorbent extraction, and sample is by filling the disposable extraction column of adsorbent, and analyte and impurity are retained on the post, remove impurity with selective solvent respectively then, and wash-out goes out analyte, thereby reaches the purpose of separation; Shortcoming is that cost is higher, and filler and eluent select to have certain difficulty, relatively is applicable to the pre-treatment experiment of predetermined substance.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method for the detection of essence gas chromatography combined with mass spectrometry is provided.
The technical solution used in the present invention is:
A kind of ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method for the detection of essence gas chromatography combined with mass spectrometry, comprise the steps: to get the essence sample in the 50mL centrifuge tube, phenixin (spreading agent) and acetone (extractant) are mixed, get mixed liquor, drawing mixed liquor injects in the centrifuge tube bottom, make it form homogeneous latex emulsion, after ultrasonic on the ultrasonic cleaner, place on the turbine mixer again and shake, it is centrifugal to take out the back, shift out subnatant, after drying up, add acetone and be settled to the laggard instrumental analysis of 1mL.
Particularly, should be used for the ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method that the essence gas chromatography combined with mass spectrometry detects, comprise the steps: to get 0.5g essence sample in the 50mL centrifuge tube, phenixin (spreading agent) and acetone (extractant) ratio according to 1:10 is mixed, get mixed liquor, drawing mixed liquor injects in the centrifuge tube bottom, make it form homogeneous latex emulsion, behind ultrasonic 10min on the ultrasonic cleaner, place again and shake 20min on the turbine mixer, take out the centrifugal 10min in back, shift out subnatant, after drying up, add acetone and be settled to the laggard instrumental analysis of 1mL.
Essence fragrance analytical approach: GC-MS analyzes
GC conditions: HB-5 capillary column (30m * 0.25 μ m * 0.25 μ m), 250 ℃ of injector temperatures, carrier gas is high-purity (〉=99.999%) helium, flow rate of carrier gas is 1.0mL/min, temperature programme: 40 ℃ of initial temperatures, keep 3.0min, 3 ℃/min rises to 80 ℃, keep 1min, rise to 230 ℃ with 15 ℃/min again and keep 10.0min.
Mass spectrum condition: EI ion gun; Electron energy 70eV; 150 ℃ of level Four bar temperature, 260 ℃ of interface temperature; Electron-multiplier voltage 1654V; 230 ℃ of ion source temperatures; The employing standard mode is tuning; Select full scan (SCAN) pattern for use, mass scanning scope: 30～550amu.
The beneficial effect that the present invention has:
The inventive method is simple, easy operating, and the time is short, and is effective.
Description of drawings
Fig. 1 is for adopting ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method of the present invention, carrying out the chromatogram that the GC-MS analytical approach obtains again to a certain essence sample.
Fig. 2 is solvent extraction method: get 0.5g essence sample in the 50mL centrifuge tube, add the 10mL ether and place and shake 20min on the turbine mixer, take out the centrifugal 10min in back, shift out clear liquid, dry up and be settled to 1mL, carry out the chromatogram that the GC-MS analytical approach obtains again.
Fig. 1 and Fig. 2 are employed to be same essence sample, and by comparative analysis as seen, the essence amount of material that the inventive method analysis obtains is many, and analysis result is more effective.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but do not limit protection scope of the present invention.
Embodiment 1
A kind of ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method for the detection of essence gas chromatography combined with mass spectrometry, comprise the steps: to get 0.5g essence sample in the 50mL centrifuge tube, phenixin (spreading agent) and acetone (extractant) ratio according to 1:10 is mixed, get mixed liquor, drawing mixed liquor injects in the centrifuge tube bottom, make it form homogeneous latex emulsion, behind ultrasonic 10min on the ultrasonic cleaner, place again and shake 20min on the turbine mixer, take out the centrifugal 10min in back, shift out subnatant, after drying up, add acetone and be settled to the laggard instrumental analysis of 1mL.
Essence fragrance analytical approach: GC-MS analyzes
GC conditions: HB-5 capillary column (30m * 0.25 μ m * 0.25 μ m), 250 ℃ of injector temperatures, carrier gas is high-purity (〉=99.999%) helium, flow rate of carrier gas is 1.0mL/min, temperature programme: 40 ℃ of initial temperatures, keep 3.0min, 3 ℃/min rises to 80 ℃, keep 1min, rise to 230 ℃ with 15 ℃/min again and keep 10.0min.
Mass spectrum condition: EI ion gun; Electron energy 70eV; 150 ℃ of level Four bar temperature, 260 ℃ of interface temperature; Electron-multiplier voltage 1654V; 230 ℃ of ion source temperatures; The employing standard mode is tuning; Select full scan (SCAN) pattern for use, mass scanning scope: 30～550amu.
Claims (2)
1. one kind is used for the ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method that the essence gas chromatography combined with mass spectrometry detects, it is characterized in that: comprise the steps: to get the essence sample in the 50mL centrifuge tube, phenixin (spreading agent) and acetone (extractant) are mixed, get mixed liquor, drawing mixed liquor injects in the centrifuge tube bottom, make it form homogeneous latex emulsion, after ultrasonic on the ultrasonic cleaner, place on the turbine mixer again and shake, it is centrifugal to take out the back, shift out subnatant, after drying up, add acetone and be settled to the laggard instrumental analysis of 1mL.
2. one kind is used for the ultrasound wave aid dispersion liquid-phase micro-extraction pre-treating method that the essence gas chromatography combined with mass spectrometry detects, it is characterized in that: comprise the steps: to get 0.5g essence sample in the 50mL centrifuge tube, phenixin (spreading agent) and acetone (extractant) ratio according to 1:10 is mixed, get mixed liquor, drawing mixed liquor injects in the centrifuge tube bottom, make it form homogeneous latex emulsion, behind ultrasonic 10min on the ultrasonic cleaner, place again and shake 20min on the turbine mixer, take out the centrifugal 10min in back, shift out subnatant, after drying up, add acetone and be settled to the laggard instrumental analysis of 1mL.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201310104973 CN103235061A (en) | 2013-03-28 | 2013-03-28 | Pretreatment method for essence gas chromatography-mass spectrometry combination detection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290663A (en) * | 2016-07-25 | 2017-01-04 | 湖北中烟工业有限责任公司 | A kind of pre-treating method of tobacco aromatics using analysis of volatile components |
| CN108828107A (en) * | 2018-09-04 | 2018-11-16 | 浙江公正检验中心有限公司 | A kind of gas chromatography combined with mass spectrometry method detecting the scented rice true and false |
-
2013
- 2013-03-28 CN CN 201310104973 patent/CN103235061A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290663A (en) * | 2016-07-25 | 2017-01-04 | 湖北中烟工业有限责任公司 | A kind of pre-treating method of tobacco aromatics using analysis of volatile components |
| CN106290663B (en) * | 2016-07-25 | 2019-02-12 | 湖北中烟工业有限责任公司 | A kind of pre-treating method of tobacco aromaticss analysis of volatile components |
| CN108828107A (en) * | 2018-09-04 | 2018-11-16 | 浙江公正检验中心有限公司 | A kind of gas chromatography combined with mass spectrometry method detecting the scented rice true and false |
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Application publication date: 20130807 |