CN104977375A - Method for determining oenanthe stolonifera D.C volatile substances - Google Patents
Method for determining oenanthe stolonifera D.C volatile substances Download PDFInfo
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- CN104977375A CN104977375A CN201510393398.4A CN201510393398A CN104977375A CN 104977375 A CN104977375 A CN 104977375A CN 201510393398 A CN201510393398 A CN 201510393398A CN 104977375 A CN104977375 A CN 104977375A
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- chinese celery
- oenanthe stolonifera
- volatile matter
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Abstract
The invention belongs to the technical fields of vegetable breeding and high-quality production, and especially relates to a method for determining oenanthe stolonifera D.C volatile substances. The method comprises the steps: cutting a fresh oenanthe stolonifera D.C sample into granules, and placing in a triangular flask; extracting the volatile substances by an extracting head; inserting the extracting head into a sample inlet of a gas chromatograph-mass spectrometer, and analyzing for 1-10 min; and separating the sample in the gas chromatograph-mass spectrometer, and acquiring data. 20-30 kinds of volatile substances can be determined from oenanthe stolonifera D.C by the method. According to the method, the extraction time and temperature are optimized, waste of the extraction time is reduced, a measured peak is single, and a peak shape is sharp, narrow and high. At the same time, with determination of the oenanthe stolonifera D.C volatile substances, a theoretical basis can be provided for oenanthe stolonifera D.C resource flavor quality identification, a basis is provided for consumers to choose oenanthe stolonifera D.C suitable for own taste, expansion of oenanthe stolonifera D.C markets is promoted, the production and sales of oenanthe stolonifera D.C is increased, and sustainable development of oenanthe stolonifera D.C industries is promoted.
Description
Technical field
The invention belongs to vegetable breeding and fine quality production technical field thereof, particularly a kind of method measuring Chinese celery volatile matter.
Background technology
Chinese celery (Oenanthe stolonifera D.C) is the perennial aquatic herbaceous plant of Carrot family, is one of important aquatic vegetable in south China area.Containing abundant dietary fiber in Chinese celery, and having effects such as promoting gastric secretion, blood circulation, increase appetite, is a kind of generally acknowledged health-care vegetable.Although Chinese celery has multiple medical value, many people are difficult to accept the peculiar taste that Chinese celery itself gives out, so many people do not have very strong wish to edible Chinese celery, this have impact on production, the popularization of Chinese celery to a certain extent.
Before making the present invention, the breed breeding of Chinese celery mainly lays particular emphasis on output and this two indices of resistance, but for the consumer in modern times, the quality of Chinese celery is even more important, not only focuses on its edibility, also focuses on its flavor quality.At present, also few to the understanding of the volatile matter determining Chinese celery flavor quality, in rearing new variety also not using the flavor quality of Chinese celery as a breeding target, cause medicinal, the nutritive value of Chinese celery itself comprehensively not to be played, have impact on consumption and the production of Chinese celery.
Summary of the invention
Object of the present invention is just to overcome above-mentioned defect, develops a kind of method measuring Chinese celery volatile matter, and for the flavor quality of Chinese celery resource is identified, the Chinese celery new varieties that seed selection meets more people's edible demand do theoretical preparation.
Technical scheme of the present invention is:
Measure a method for Chinese celery volatile matter, its technical characteristics step is as follows:
(1) fresh Chinese celery is cut into graininess, is placed in triangular flask;
(2) volatile matter is extracted with solid phase micro-extraction technique;
(3) injection port extracting head being inserted gas chromatograph-mass spectrometer is resolved;
(4) sample separation in gas chromatograph-mass spectrometer, image data.
Described step is as follows:
(1) take 1 ?15g chopping fresh mature Chinese celery, be placed in triangular flask;
(2) extract by the extracting head of 65 μm of PDMS/DVB, 70 μm of CW/DVB, 75 μm of Carboxen/PDMS, 100 μm of PDMS respectively;
(3) 20 ?extract in the thermostat water bath of 70 DEG C 5 ?80min;
(4) the injection port of gas chromatograph-mass spectrometer resolve 1 ?10min;
(5) gas chromatography mass spectrometry condition: DB ?5MS (30m × 0.25mm × 0.25 μm) capillary chromatographic column, carrier gas He, flow velocity is 1mL/min, split ratio be 4:1 ?50:1, injector temperature 250 DEG C, post heating schedule: initial temperature 50 DEG C, keeps 2min, 10 DEG C/min rises to 95 DEG C, then rises to 300 DEG C with 5 DEG C/min.Ion source temperature 200 DEG C, ionization mode EI, EI source temperature 250 DEG C, transmission line temperature 250 DEG C, electron energy 70eV, detector voltage 350V, quality surface sweeping scope 10 ?600amu.
Described step (4) resolves 2min at injection port.
Described step (1) takes 2g graininess fresh mature Chinese celery, by the extracting head of 70 μm of CW/DVB in step (2), extracts 20min in step (3) in the thermostat water bath of 35 DEG C.
Described step (1) takes 7g graininess fresh mature Chinese celery, by the extracting head of 100 μm of PDMS in step (2), extracts 33min in step (3) in the thermostat water bath of 40 DEG C.
Advantage of the present invention and effect there are provided a kind of method of mensuration Chinese celery volatile matter of a complete set.Utilize this method can determine from Chinese celery 20 ?30 kinds of volatile matter.This method is optimized on extraction time and temperature, decreases the waste of extraction time, and the peak measured is single, and peak shape is sharp, narrow, high.Meanwhile, the mensuration of Chinese celery volatile matter, can provide fundamental basis for the qualification of Chinese celery resource flavor quality, for consumer provides foundation on the Chinese celery selecting oneself taste applicable, promote the expansion in Chinese celery market, increase turnout and the sale of Chinese celery, promote the sustainable development of Chinese celery industry.The mensuration of Chinese celery volatile matter, also for Chinese celery breed breeding has expanded direction, has been broken traditional breed breeding being leading indicator with output and resistance, will have been promoted Chinese celery quality breeding process.Therefore, the present invention not only theoretical and technically have new breakthrough, and can promote Chinese celery industry development, lifting economic and social benefits and ecological benefits.
Of the present invention other advantage and effect will go on to say below more specifically.
Embodiment
Technical thought of the present invention is:
A kind of method measuring Chinese celery volatile matter is provided, thus for providing fundamental basis in the flavor quality qualification of Chinese celery resource, promotes the breeding of Chinese celery flavor quality, promoting the development of Chinese celery industry.
Illustrate the present invention below.
Embodiment 1:
Get fresh mature Chinese celery, clean, be cut into graininess, take 2g and be placed in triangular flask, with aluminium-foil paper and sealed membrane sealing, aging 70 μm of good CW/DVB extracting head are inserted triangular flask head space part, release fiber head, be fixed in the thermostat water bath of 35 DEG C, extraction 20min, after having extracted, regain fiber head, extract extracting head, then extracting head is inserted the injection port of gas chromatograph-mass spectrometer, release fiber head, resolve 2min, extract extracting head.Gas chromatography mass spectrometry condition: DB ?5MS (30m × 0.25mm × 0.25 μm) capillary chromatographic column, carrier gas He, flow velocity is 1mL/min, split ratio is 5:1, injector temperature 250 DEG C, post heating schedule: initial temperature 50 DEG C, keeps 2min, 10 DEG C/min rises to 95 DEG C, then rises to 300 DEG C with 5 DEG C/min.Ion source temperature 200 DEG C, ionization mode EI, EI source temperature 250 DEG C, transmission line temperature 250 DEG C, electron energy 70eV, detector voltage 350V, quality surface sweeping scope 23 ?350amu, by this program sample separation, image data, separablely obtain 10 kinds of Chinese celery volatile matter, the volatile matter of 54% can be separated completely.
Embodiment 2:
Get fresh mature Chinese celery, clean, be cut into graininess, take 7g and be placed in triangular flask, with aluminium-foil paper and sealed membrane sealing, aging 100 μm of good CW/DVB extracting head are inserted triangular flask head space part, release fiber head, be fixed in the thermostat water bath of 40 DEG C, extraction 33min, after having extracted, regain fiber head, extract extracting head, then extracting head is inserted the injection port of gas chromatograph-mass spectrometer, release fiber head, resolve 2min, extract extracting head.Gas chromatography mass spectrometry condition: DB ?5MS (30m × 0.25mm × 0.25 μm) capillary chromatographic column, carrier gas He, flow velocity is 1mL/min, split ratio is 14:1, injector temperature 250 DEG C, post heating schedule: initial temperature 50 DEG C, keeps 2min, 10 DEG C/min rises to 95 DEG C, then rises to 300 DEG C with 5 DEG C/min.Ion source temperature 200 DEG C, ionization mode EI, EI source temperature 250 DEG C, transmission line temperature 250 DEG C, electron energy 70eV, detector voltage 350V, quality surface sweeping scope 33 ?350amu, by this program sample separation, image data, separablely obtain 17 kinds of Chinese celery volatile matter, the volatile matter of 50% can be separated completely.
Embodiment 3:
Get fresh mature Chinese celery, clean, be cut into graininess, take 10g and be placed in triangular flask, with aluminium-foil paper and sealed membrane sealing, aging 65 μm of good CW/DVB extracting head are inserted triangular flask head space part, release fiber head, be fixed in the thermostat water bath of 45 DEG C, extraction 15min, after having extracted, regain fiber head, extract extracting head, then extracting head is inserted the injection port of gas chromatograph-mass spectrometer, release fiber head, resolve 2min, extract extracting head.Gas chromatography mass spectrometry condition: DB ?5MS (30m × 0.25mm × 0.25 μm) capillary chromatographic column, carrier gas He, flow velocity is 1mL/min, split ratio is 65.1:1, injector temperature 250 DEG C, post heating schedule: initial temperature 50 DEG C, keeps 2min, 10 DEG C/min rises to 95 DEG C, then rises to 300 DEG C with 5 DEG C/min.Ion source temperature 200 DEG C, ionization mode EI, EI source temperature 250 DEG C, transmission line temperature 250 DEG C, electron energy 70eV, detector voltage 350V, quality surface sweeping scope 45 ?450amu, by this program sample separation, image data, separablely obtain 20 kinds of Chinese celery volatile matter, the volatile matter of 65% can be separated completely.
Embodiment 4:
Get fresh mature Chinese celery, clean, be cut into graininess, take 11g and be placed in triangular flask, with aluminium-foil paper and sealed membrane sealing, aging 75 μm of good CW/DVB extracting head are inserted triangular flask head space part, release fiber head, be fixed in the thermostat water bath of 55 DEG C, extraction 40min, after having extracted, regain fiber head, extract extracting head, then extracting head is inserted the injection port of gas chromatograph-mass spectrometer, release fiber head, resolve 2min, extract extracting head.Gas chromatography mass spectrometry condition: DB ?5MS (30m × 0.25mm × 0.25 μm) capillary chromatographic column, carrier gas He, flow velocity is 1mL/min, split ratio is 50:1, injector temperature 250 DEG C, post heating schedule: initial temperature 50 DEG C, keeps 2min, 10 DEG C/min rises to 95 DEG C, then rises to 300 DEG C with 5 DEG C/min.Ion source temperature 200 DEG C, ionization mode EI, EI source temperature 250 DEG C, transmission line temperature 250 DEG C, electron energy 70eV, detector voltage 350V, quality surface sweeping scope 50 ?500amu, by this program sample separation, image data, separablely obtain 24 kinds of Chinese celery volatile matter, the volatile matter of 85% can be separated completely.
Claims (5)
1. measure a method for Chinese celery volatile matter, it is characterized in that step is as follows:
(1) fresh Chinese celery sample is cut into graininess, is placed in triangular flask;
(2) volatile matter is extracted by extracting head;
(3) injection port extracting head being inserted gas chromatograph-mass spectrometer carry out parsing 1 ?10min;
(4) sample separation in gas chromatograph-mass spectrometer, image data.
2. a kind of method measuring Chinese celery volatile matter according to claim 1, is characterized in that step is as follows:
(1) take the fresh Chinese celery sample that 1 ?15g shreds, be placed in triangular flask;
(2) extract by the extracting head of 65 μm of PDMS/DVB or 70 μm CW/DVB or 75 μm Carboxen/PDMS or 100 μm PDMS; 20 ?extract in the thermostat water bath of 70 DEG C 5 ?80min;
(3) injection port extracting head being inserted gas chromatograph-mass spectrometer resolve 1 ?10min;
(4) gas chromatography mass spectrometry condition: DB ?5MS 30m × 0.25mm × 0.25 μm capillary chromatographic column, carrier gas He, flow velocity is 1mL/min, split ratio be 4:1 ?50:1, injector temperature 250 DEG C, post heating schedule: initial temperature 50 DEG C, keeps 2min, with 3 ?15 DEG C/min rise to 85 ?155 DEG C, then with 5 ?20 DEG C/min rise to 175 ?300 DEG C.Ion source temperature 200 DEG C, ionization mode EI, EI source temperature 250 DEG C, transmission line temperature 250 DEG C, electron energy 70eV, detector voltage 350V, quality surface sweeping scope 10 ?600amu.
3. a kind of method measuring Chinese celery volatile matter according to claim 2, is characterized in that step (3) resolves 2min at injection port.
4. a kind of method measuring Chinese celery volatile matter according to claim 2, it is characterized in that step (1) takes the fresh Chinese celery sample of 2g chopping, by the extracting head of 70 μm of CW/DVB in step (2), in the thermostat water bath of 35 DEG C, extract 20min.
5. a kind of method measuring Chinese celery volatile matter according to claim 2, it is characterized in that step (1) takes 7g graininess fresh mature Chinese celery, by the extracting head of 100 μm of PDMS in step (2), in the thermostat water bath of 40 DEG C, extract 33min.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104316635A (en) * | 2014-10-28 | 2015-01-28 | 石河子大学 | Method for rapidly identifying flavor and quality of fruits |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104316635A (en) * | 2014-10-28 | 2015-01-28 | 石河子大学 | Method for rapidly identifying flavor and quality of fruits |
Non-Patent Citations (3)
| Title |
|---|
| DENG, CH; SONG, GX; ZHENG, XH: "Analysis of the volatile constituents of Apium graveolens L. and Oenanthe L. by gas chromatography-mass spectrometry, using headspace solid-phase microextraction", 《CHROMATOGRAPHIA》 * |
| 王润贤: "春秋季节不同品种茶鲜叶芳香物质成分分析", 《山西农业大学学报》 * |
| 章宏慧: "不同加工方式对水芹挥发性成分的影响", 《中国食品学报》 * |
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Application publication date: 20151014 |