CN103837622A - Method for rapidly identifying types of tea oil - Google Patents
Method for rapidly identifying types of tea oil Download PDFInfo
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- CN103837622A CN103837622A CN201410108982.6A CN201410108982A CN103837622A CN 103837622 A CN103837622 A CN 103837622A CN 201410108982 A CN201410108982 A CN 201410108982A CN 103837622 A CN103837622 A CN 103837622A
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Abstract
The invention discloses a method for rapidly identifying types of tea oil. The method comprises the following steps: selecting tea oil with representativeness in a processing technology as a standard sample, adsorbing volatile components of the tea oil by using a fiber head, separating the volatile components by adopting a gas chromatograph equipped with a FID detector, measuring, generating a common mode chromatogram map by utilizing a chromatographic fingerprint similarity evaluation system, determining the similarity of the tea oil in the processing technology relative to the common mode chromatogram map, evaluating the similarity of a chromatogram map of the volatile components of the tea oil relative to the common mode chromatogram map, comparing the similarity of the volatile components of the tea oil with the similarity of the tea oil in each processing technology to finish identification of the types of the tea oil. The method is simple to operate and high in accuracy, and the tea oil in different processing technologies can be identified.
Description
Technical field
The present invention relates to tea oil detection field, particularly relate to and a kind of analyze tea oil volatile ingredient by gas chromatograph and differentiate fast tea oil class method for distinguishing.
Technical background
The processing technology of tea oil directly affects the quality of tea oil, and its market price of the tea oil of different processing technologys has very big-difference, and therefore the discrimination method of tea oil classification is significant in tea oil intermediate links.Classic method is to differentiate tea oil classification with sensory evaluation (as color and luster, smell, flavour), but selectivity is not strong, easily causes deviation; And different processing technology means can cause tea oil to have very big-difference on volatile ingredient composition, therefore existing tea oil analytical approach lacks the tea oil of differentiating different processing technologys.
Summary of the invention
Technical matters to be solved by this invention is, overcomes the above-mentioned deficiency of prior art, provides one to differentiate fast simply accurately tea oil class method for distinguishing, can realize the tea oil of different processing technologys and differentiate.
The technical scheme that the present invention solves its technical matters employing is: a kind of tea oil class method for distinguishing of differentiating fast, comprises the following steps:
(1) tea oil sampling: choose the representative tea oil of processing technology as the standard model in method database;
(2) volatile ingredient extraction: take 0.19 g tea oil and 0.01 g internal standard compound dodecane is placed in 15 mL head space bottles, sealing rapidly, under 95 ℃ of conditions, heat, after reprocess fibre head adsorb volatile composition 10 min, deliver to rapidly gas phase injection port and resolve 10 min;
(3) GC analyzes: adopt gas chromatograph to be equipped with fid detector volatile ingredient is separated, measure, obtain tea oil volatile ingredient chromatogram; The condition of gas chromatograph is: nitrogen buffer gas, injection port and detector temperature are 250 ℃, sample introduction is not shunted, column oven heating schedule is: initial temperature is 40 ℃, keep 2 min, be then warming up to 160 ℃ with the speed of 3.00 ℃/min, keep 2 min, be warming up to 220 ℃ with the speed of 12 ℃/min again, keep 5 min; After mensuration, continue sample introduction, until obtain the tea oil volatile ingredient chromatogram of all processing technologys;
(4) common pattern chromatogram generates: utilize chromatographic fingerprinting similarity evaluation system, the tea oil chromatogram of all processing technologys is analyzed, and then generate common pattern chromatogram;
(5) tea oil similarity is established: take common pattern chromatogram as standard spectrogram, the tea oil chromatogram of different processing technologys and common pattern chromatogram are compared respectively, and determine the similarity of each processing technology tea oil by chromatographic fingerprinting similarity evaluation system;
(6) sample analysis: utilize chromatographic fingerprinting similarity evaluation system, take the each chromatographic peak in tea oil volatile ingredient chromatogram with respect to the retention time at interior mark peak and peak area as parameter, with the common pattern chromatogram calculating similarity of comparing, and the similarity calculating and each processing technology tea oil similarity are compared, thereby determine this tea oil classification.
Further, in step (1), choose tea oil that coarse tea oil, refining tea oil and water that hot moulding, cold press, extraction produce produces for centrifuging as the standard model in method database.
Further, in step (2), take 0.19 g tea oil and 0.01 g internal standard compound dodecane is placed in 15 mL head space bottles, rapidly with sealing with the bottle cap of teflon gasket, under 95 ℃ of conditions, heat, then resolve 10 min with delivering to rapidly gas phase injection port after DVB/CAR/PDMS 50/30 μ m fiber head adsorb volatile composition 10 min.
Further, in step (3), adopt SP2340, the gas chromatograph of 60 mm × 0.2, m × 0.25 μ m film thickness Fused-silica capillary columns is equipped with fid detector volatile ingredient is separated, and measures.
Further, in step (6), described similarity is obtained by following formula,
In formula, X is the finger-print vector of tea oil volatile ingredient, the finger-print vector that Y is common pattern.
The beneficial effect that the present invention compared with prior art has:
1. the accuracy of analyzing: utilizing gas chromatograph to be equipped with fid detector can separate completely to the volatile ingredient in tea oil, and obtain the relative content of the each composition of volatile matter, thereby improve the accuracy of analyzing, this is incomparable in organoleptic analysis;
2. applicable popularity and simplicity: the method for setting up can be differentiated the tea oil that coarse tea oil, refining tea oil and the water of hot moulding, cold press, extraction production are produced for centrifuging; The detection of oil sample must not carried out complicated pre-service;
3. the data of a method for building up are stored in working software and can use for a long time, must calibration.
annex explanation
Fig. 1 is the different processing technology tea oil of embodiment of the present invention chromatogram;
Fig. 2 is the different processing technology tea oil of embodiment of the present invention sample common pattern chromatogram;
Fig. 3 is cold press refining tea oil volatile ingredient chromatogram and the common pattern chromatogram of embodiment 1;
Fig. 4 is cold press coarse tea oil volatile ingredient chromatogram and the common pattern chromatogram of embodiment 2;
Fig. 5 is hot moulding coarse tea oil volatile ingredient chromatogram and the common pattern chromatogram of embodiment 3;
Fig. 6 is hot moulding refining tea oil volatile ingredient chromatogram and the common pattern chromatogram of embodiment 4;
Fig. 7 is extraction coarse tea oil volatile ingredient chromatogram and the common pattern chromatogram of embodiment 5;
Fig. 8 is refined extraction tea oil volatile ingredient chromatogram and the common pattern chromatogram of embodiment 6;
Fig. 9 is that the water of embodiment 7 is for centrifuging tea oil volatile ingredient chromatogram and common pattern chromatogram.
Embodiment
The one that the present embodiment provides is differentiated tea oil class method for distinguishing fast, to utilize gas chromatograph to set up the common pattern chromatogram of four class processing technology tea oil, the chromatographic fingerprinting similarity evaluation system of using the mathematical statistics method such as PCA to set up, the similarity take sample volatile ingredient chromatogram than common pattern chromatogram is differentiated the tea oil of different processing technologys as index.
The present embodiment comprises the following steps:
(1) tea oil sampling: choose tea oil that coarse tea oil, refining tea oil and water that hot moulding, cold press, extraction produce produces for centrifuging as the standard model in method database, specifically choose hot moulding, cold press, extraction and water and choose at random again 3 kinds of generic tea oil for four kinds of processing technologys of centrifuging, same processing technology, totally 21 kinds of tea oil as standard model;
(2) volatile ingredient extraction: a certain processing technology tea oil and the 0.01 g dodecane got in 0.19 g standard model are placed in 15 mL head space bottles rapidly with sealing with the bottle cap of teflon gasket, under 95 ℃ of conditions, heat, then resolve 10 min with delivering to rapidly gas phase injection port after DVB/CAR/PDMS 50/30 μ m fiber head adsorbing volatilizing thing 10 min;
(3) GC analyzes: adopt the gas chromatograph outfit fid detector of SP2340 (60 mm × 0.2, m × 0.25 μ m film thickness) Fused-silica capillary column to separate volatile ingredient, measure, obtain this tea oil volatile ingredient chromatogram; The condition of gas chromatograph is: nitrogen is as carrier gas, injection port and detector temperature are 250 ℃, sample introduction is not shunted, column oven heating schedule is: initial temperature is 40 ℃, keep 2 min, be then warming up to 160 ℃ with the speed of 3.00 ℃/min, keep 2 min, be warming up to 220 ℃ with the speed of 12 ℃/min again, keep 5 min; After mensuration, continue sample introduction, until obtain 21 kinds of tea oil volatile ingredient chromatograms;
(4) common pattern chromatogram generates: utilize chromatographic fingerprinting similarity evaluation system, 21 kinds of tea oil chromatograms are analyzed, and then generate common pattern chromatogram, see figures.1.and.2; 21 kinds of tea oil chromatograms in Fig. 1 are followed successively by sample 1-21(from top to bottom with reference to table 1);
(5) tea oil similarity is established: take common pattern chromatogram as standard spectrogram, 21 kinds of tea oil chromatograms and common pattern chromatogram are compared respectively, and determine the similarity of 21 kinds of tea oil and the similarity scope of 7 kinds of different processing technology tea oil by chromatographic fingerprinting similarity evaluation system, with reference to table 1;
(6) sample analysis: utilize chromatographic fingerprinting similarity evaluation system, take the each chromatographic peak in tea oil volatile ingredient chromatogram with respect to the retention time at interior mark peak and peak area as parameter, compare with common pattern chromatogram, adopt Cosin method to calculate similarity, and tea oil similarity scope in the similarity calculating and table 1 is compared, thereby determine this tea oil classification.
Wherein, similarity is obtained by following formula,
In formula, X is the finger-print vector of tea oil volatile ingredient, the finger-print vector that Y is common pattern.
The present embodiment has been chosen volatile ingredient chromatogram and the common pattern chromatogram of the tea oil of 9 kinds of different processing technologys and has been compared, to determine similarity, with reference to Fig. 3 ~ Fig. 9.Wherein, the R (5) in Fig. 3 ~ Fig. 9 represents common pattern chromatogram, and S2 (5) represents tea oil sample volatile ingredient chromatogram.
In Fig. 3, calculating similarity by analytic system is 0.581, in cold press refining tea oil similarity interval (0.564,0.594), so this tea oil is defined as cold press refining tea oil.
In Fig. 4, calculating similarity by analytic system is 0.718, in cold press coarse tea oil similarity interval (0.703,0.727), so this tea oil is defined as cold press coarse tea oil.
In Fig. 5, calculating similarity by analytic system is 0.902, in hot moulding coarse tea oil similarity interval (0.872,0.910), so this tea oil is defined as hot moulding coarse tea oil.
In Fig. 6, calculating similarity by analytic system is 0.808, in hot moulding refining tea oil similarity interval (0.802,0.822), so this tea oil is defined as hot moulding refining tea oil.
In Fig. 7, calculating similarity by analytic system is 0.775, in extraction coarse tea oil similarity interval (0.766,0.794), so this tea oil is defined as extraction coarse tea oil.
In Fig. 8, calculating similarity by analytic system is 0.439, in refined extraction tea oil similarity interval (0.423,0.455), so this tea oil is defined as refined extraction tea oil.
In Fig. 9, calculating similarity by analytic system is 0.960, in water for centrifuging tea oil similarity interval (0.947,0.963), so this tea oil is defined as water for centrifuging tea oil.
Claims (6)
1. differentiate fast a tea oil class method for distinguishing, it is characterized in that, comprise the steps:
(1) tea oil sampling: choose the representative tea oil of processing technology as the standard model in method database;
(2) volatile ingredient extraction: take 0.19 g tea oil and 0.01 g internal standard compound dodecane is placed in 15 mL head space bottles, sealing rapidly, under 95 ℃ of conditions, heat, after reprocess fibre head adsorb volatile composition 10 min, deliver to rapidly gas phase injection port and resolve 10 min;
(3) GC analyzes: adopt gas chromatograph to be equipped with fid detector volatile ingredient is separated, measure, obtain tea oil volatile ingredient chromatogram; The condition of gas chromatograph is: nitrogen buffer gas, injection port and detector temperature are 250 ℃, sample introduction is not shunted, column oven heating schedule is: initial temperature is 40 ℃, keep 2 min, be then warming up to 160 ℃ with the speed of 3.00 ℃/min, keep 2 min, be warming up to 220 ℃ with the speed of 12 ℃/min again, keep 5 min; After mensuration, continue sample introduction, until obtain the tea oil volatile ingredient chromatogram of all processing technologys;
(4) common pattern chromatogram generates: utilize chromatographic fingerprinting similarity evaluation system, the tea oil chromatogram of all processing technologys is analyzed, and then generate common pattern chromatogram;
(5) tea oil similarity is established: take common pattern chromatogram as standard spectrogram, the tea oil chromatogram of different processing technologys and common pattern chromatogram are compared respectively, and determine the similarity of each processing technology tea oil by chromatographic fingerprinting similarity evaluation system;
(6) sample analysis: utilize chromatographic fingerprinting similarity evaluation system, take the each chromatographic peak in tea oil volatile ingredient chromatogram with respect to the retention time at interior mark peak and peak area as parameter, with the common pattern chromatogram calculating similarity of comparing, and the similarity calculating and each processing technology tea oil similarity are compared, thereby determine this tea oil classification.
2. differentiate fast according to claim 1 tea oil class method for distinguishing, it is characterized in that, in step (1), choose tea oil that coarse tea oil, refining tea oil and water that hot moulding, cold press, extraction produce produces for centrifuging as the standard model in method database.
3. according to differentiating fast tea oil class method for distinguishing described in claim 1 or 2, it is characterized in that, in step (2), take 0.19 g tea oil and 0.01 g internal standard compound dodecane is placed in 15 mL head space bottles, rapidly with sealing with the bottle cap of teflon gasket, under 95 ℃ of conditions, heat, then resolve 10 min with delivering to rapidly gas phase injection port after DVB/CAR/PDMS 50/30 μ m fiber head adsorb volatile composition 10 min.
4. according to differentiating fast tea oil class method for distinguishing described in claim 1 or 2, it is characterized in that, in step (3), adopt SP2340, the gas chromatograph of 60 mm × 0.2, m × 0.25 μ m film thickness Fused-silica capillary columns is equipped with fid detector volatile ingredient is separated, and measures.
5. differentiate fast according to claim 3 tea oil class method for distinguishing, it is characterized in that, in step (3), adopt SP2340, the gas chromatograph of 60 mm × 0.2, m × 0.25 μ m film thickness Fused-silica capillary columns is equipped with fid detector volatile ingredient is separated, and measures.
6. it is characterized in that tea oil class method for distinguishing according to differentiating fast described in claim 1 or 2, in step (6), described similarity is obtained by following formula,
In formula, X is the finger-print vector of tea oil volatile ingredient, the finger-print vector that Y is common pattern.
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| CN106483238A (en) * | 2015-11-16 | 2017-03-08 | 苏州云溪分析技术有限公司 | A kind of method of Rapid identification oil types |
| CN108845045A (en) * | 2018-05-03 | 2018-11-20 | 北京工商大学 | A kind of method that gas-phase fingerprint pattern combination principal component analytical method differentiates frying oil quality |
| CN113759032A (en) * | 2021-06-28 | 2021-12-07 | 河南工业大学 | Oil and fat blending identification method |
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| CN106483238A (en) * | 2015-11-16 | 2017-03-08 | 苏州云溪分析技术有限公司 | A kind of method of Rapid identification oil types |
| CN108845045A (en) * | 2018-05-03 | 2018-11-20 | 北京工商大学 | A kind of method that gas-phase fingerprint pattern combination principal component analytical method differentiates frying oil quality |
| CN113759032A (en) * | 2021-06-28 | 2021-12-07 | 河南工业大学 | Oil and fat blending identification method |
| CN113759032B (en) * | 2021-06-28 | 2023-04-18 | 河南工业大学 | Oil and fat blending identification method |
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Application publication date: 20140604 |