CN104034836A - Method for detecting olefin components in orange juice by applying on-line solid-phase microextraction method and comprehensive two-dimensional gas chromatography-quadrupole mass spectrography - Google Patents
Method for detecting olefin components in orange juice by applying on-line solid-phase microextraction method and comprehensive two-dimensional gas chromatography-quadrupole mass spectrography Download PDFInfo
- Publication number
- CN104034836A CN104034836A CN201410232628.4A CN201410232628A CN104034836A CN 104034836 A CN104034836 A CN 104034836A CN 201410232628 A CN201410232628 A CN 201410232628A CN 104034836 A CN104034836 A CN 104034836A
- Authority
- CN
- China
- Prior art keywords
- gas chromatography
- comprehensive
- olefines
- component
- dimensional gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for authenticating and analyzing olefin components in orange juice by applying an on-line solid-phase microextraction (online-SPME) method and a comprehensive two-dimensional gas chromatography-quadrupole mass spectrography (Comprehensive2DGC/qMS). The olefin components in an orange juice sample are enriched by on-line solid-phase microextraction and are detected by adopting a comprehensive two-dimensional gas chromatography-quadrupole mass spectrography; detected compounds are qualitatively analyzed in a mode of combining a retention index and an NIST spectrum library, and overlapped chromatographic peaks in the components which cannot be separated by adopting the comprehensive two-dimensional gas chromatography are accurately quantified by adopting section convolution pairs; the olefin components are subjected to orthogonal separation by adopting two chromatographic columns with different polarities by the comprehensive two-dimensional gas chromatography; under the action of a modulator-demodulator, the olefin components are detected by adopting the quadrupole mass spectrography; the qualitative analysis is performed in a mode of combining a retention time index and the NIST spectrum library; the overlapped chromatographic peaks are accurately quantified by adopting a section convolution technology. The method disclosed by the invention has the characteristics of high flux, high sensitivity and high accuracy; the problems of difficulty in analysis and separation of the olefin components in the orange juice and difficulty in qualification can be solved.
Description
Technical field
The invention belongs to food security technical field, relate to a kind of method of applying olefines component in online solid-phase microextraction and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy detection orange juice.
Background technology
Orange juice is nutritious, and taste-aromatic is pleasant, is the drink variety that the whole world is rather well received, consumption figure is large.Wherein orange juice is at the forefront in the world as its consumption figure position of main orange juice drink.In recent years, orange juice and beverage industry thereof be along with the raising of people's degree of recognition gets a larger development, but due to the shortage of the respective quality hierarchy of control, its quality is adulterated, deception, objectionable impurities exceed standard etc., phenomenon still happens occasionally.
GB mainly comprises basic physical and chemical index for the monitoring of orange juice safety at present, as ratio and the patulin of regulation soluble solid, sucrose, glucose, fructose and glucose/fructose and orange juice content in GB/T 21731-2008 " orange juice and orange beverage ", so main focus also concentrates on basic physical and chemical index, residues of pesticides and microbiological indicator aspect, as recorded agricultural chemicals severe overweight in " Finda series " orange juice in 2009 and lemon beverage; State General Administration for Quality Supervision spot-check approximately 2% orange beverage and exceeded standard defective because of total plate count, Molds and yeasts number to 160 kinds of fruit and vegetable juice products in August, 2011; At the beginning of 2012, the Brazilian orange juice that Coca-Cola is produced contains a small amount of carbendazim agricultural chemicals etc.But do not deal with the adulterated of orange juice industry existence and blend phenomenon for quality standard or the examination criteria system of orange juice quality.The appearance of Taiwan beverage plasticiser event in 2011 also reflects the disappearance of domestic orange juice character surveillance system, and therefore studying aromatised fraction in orange juice is the basis of setting up orange juice quality standard, significant to the monitoring of orange juice quality.In orange juice, olefines component is the important component part of fragrance ingredient in orange juice.The fragrance of orange juice is had to important contribution.
Comprehensive two dimensional gas chromatography-level Four bar analytical technique of mass spectrum is the two dimensional separation by two different and separate separating mechanism chromatographic columns are combined to realize olefines material in the mode of series connection, between these two chromatographic columns, modulator is housed, modulator plays trapping and transmits.In GC × GC, the separation mechanism of two pillars is separate, each cut after the 1st chromatographic column separates, all be introduced into modulator, after focusing on, be sent to the 2nd chromatographic column with pulse mode again and carry out further compartment analysis, each cut is wanted to be eluted and is entered the 2nd root chromatogram column simultaneously, thereby in order to avoid affects separation efficiency with other cut generation co-elutes.
In existing detection fruit juice, the method for olefines material adopts traditional one dimension gas chromatography-mass spectrography, the separating power of one dimension gas chromatography is limited, cannot make all components separate completely, single analyses may can only be analyzed tens kinds of compounds, and comprehensive two dimensional gas chromatography-level Four bar analytical technique of mass spectrum detection compound can reach hundreds of, its peak capacity is that the hundreds of of one dimension liquid chromatography-mass spectrography arrives several thousand times.Adopt two-dimensional quadrature separation, the component that cannot separate in one dimension gas chromatography well can have been separated, greatly improved separation efficiency.
Summary of the invention
The problem existing for prior art, the object of the invention is to design the method that provides the online solid-phase microextraction of application of a kind of high flux, high sensitivity, good separating effect and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy to detect olefines component in orange juice.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of applying olefines component in online solid-phase microextraction and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy detection orange juice, comprises the following steps:
1) the olefines component in orange juice adopts online solid-phase microextraction Extraction and enrichment;
2) adopt comprehensive two dimensional gas chromatography to carry out orthogonal separation, level Four bar mass spectrum detects;
3) mode of the qualitative employing retention time of olefines component exponential sum NIST spectrum storehouse combination;
4) by joint convolution technique, chromatogram peak purity is judged, carry out accurate quantitative analysis analysis for chromatogram overlap peak by different choice ion.
Specifically, comprise the following steps:
1) the olefines component in orange juice adopts online solid-phase microextraction Extraction and enrichment
Take the fresh squeezing orange juice of 5 g in 10 mL headspace sampling bottles, add 2 g NaCl, seal.Adopt full-automatic solid-phase microextraction and full-automatic input mode to carry out the sorption and desorption of sample.
Online solid-phase microextraction condition is: extracting head is 85 μ m Polyacrylate self-action extracting head; Sample incubation temperature is 45
oc; Hatching balance 10 min; It is 12 mm that extracting head is inserted the sample bottle degree of depth; Extraction time is 20 min.
2) adopt comprehensive two dimensional gas chromatography-level Four bar Mass Spectrometer Method
Use comprehensive two dimensional gas chromatography-level Four bar mass spectrometer to detect olefines component: by Using Automated Solid Phase Microextraction adsorption and enrichment olefines component, being adsorbed in the mode that the determinand in extracting head analyses by pyrolysis at injection port enters in comprehensive two dimensional gas chromatography-level Four bar mass spectrometer, component to be measured is after one dimension chromatographic column separates, after modulator-demodular unit heating is cooling, enter two-dimensional gas chromatography post and separate again, detect by level Four bar mass spectrum full scan.
3) olefines component qualitative analysis
A) data analysis adopts GC image version 2.3;
B) the n-alkane standard items of C8-C20, adopt gas sampling pattern, utilize comprehensive two dimensional gas chromatography-level Four bar mass spectrum to analyze, obtain the retention time of C8-C20 n-alkane in a peacekeeping two dimension, the retention time index of the n-alkane of artificial definition C8-C20, the n-alkane retention time Index Definition that is 8 as atom number is 800, by that analogy (C atom number × 100).
C) according to the retention time index of the retention time calculating target compound of olefines component.
D) in the time that sample ionizes under the condition of EI ionization source 0.9kv voltage, its mass spectrogram and NIST spectrum storehouse compare, and when similarity is greater than setting value, this material is automatically recognized.
E) carry out qualitative in conjunction with retention time exponential sum NIST spectrum library searching result to olefines component.
4) quantitative test of olefines component
A) directly record peak area for the good olefines component of degree of separation.
B) for chromatogram overlap peak, adopt joint convolution technique to judge peak purity, when judging what peak overlapped to form as various ingredients, survey by selecting ionic means to distinguish quantitative test to overlap peak.
Described step 1) adopts online solid-phase microextraction to carry out the pre-treatment of sample.
Described step 2) adopt comprehensive two dimensional gas chromatography-level Four bar mass spectrum to detect.
In described step 3), adopt the mode that retention time index is combined with NIST spectrum storehouse to carry out qualitative analysis.
Described step 4) adopts joint convolution technique to carry out accurate quantitative analysis to chromatogram overlap peak.
Comprehensive two dimensional gas chromatography condition in described step 4):
One dimension chromatographic column is non-polar column DB-1 15m × 0.25mm × 0.1 μ m;
Two dimension chromatographic column is polar column BPX-50 15m × 0.1mm × 0.1 μ m;
Carrier gas: He, flow velocity 1.0 ml/mL;
Sampling condition: injection port resolution temperature is 250
oc, resolves 5 min.Injector temperature is 250
oc;
Column oven heating schedule: initial temperature is 35
oc, keeps 1 min, then with 3
othe heating rate of C/min is warming up to 270
oc, keeps 5 min;
Modulator-demodular unit arranges: be 6 s modulation period; Cold spray air flow is 10 mL/min; The jet temperature of heat is 325
oc, the heat spray duration is 350 ms;
Mass spectrum condition: mass detector is level Four bar mass spectrum; Ion source temperature 230
oc; Interface temperature 280
oc; Solvent delay 3 min; Adopt full scan mode, sweep limit is 30 m/z-300 m/z, sweep frequency: 20000 Hz.
Advantage of the present invention and good effect are as follows:
(1) one dimension gas chromatography chromatographic column can only be that a kind of polarity is as nonpolar or polarity, and two-dimensional gas chromatography can use nonpolar and polar column simultaneously, when multiple determinand process one dimension non-polar column, first separate by molecular size, during again through two-dimentional polarity chromatographic column, again separate by polarity again, therefore can reach the separating effect of GC × GC, complex matrices can efficiently be separated, therefore the inventive method is applicable to constituent analysis, has absolute advantage for the olefines component of analyzing in orange juice;
(2) unknown material is qualitative conventionally by means of standard substance, along with the raising of instrumental analysis ability, also can carry out qualitative analysis by means of high resolution mass spectrum.But for constituent analysis, component to be analyzed has hundreds of conventionally, the qualitative mode of standard substance and high resolution mass spectrum can more consuming time, cost.Therefore the present invention is applied to retention time index the qualitative analysis of comprehensive two dimensional gas chromatography data: in the time that chromatographic column is identical with chromatographic condition, the retention time index of material becomes to have correlativity with C atom number.The present invention adopts retention time index to carry out qualitative analysis with the mode that NIST spectrum storehouse combines.
(3) comprehensive two dimensional gas chromatography is because its separate substance kind is more, the mass spectrum of the high sweep velocity that need to match, the level Four bar mass spectrum that the present invention uses has been abandoned the low shortcoming of traditional level Four bar scanning of the mass spectrum speed, its sweep speed can reach 30000Hz, can meet the demand of comprehensive two dimensional gas chromatography to sweep velocity.
Brief description of the drawings
Fig. 1 is comprehensive two dimensional gas chromatography-level Four bar mass spectrogram of olefines material in orange juice sample;
Fig. 2 is comprehensive two dimensional gas chromatography-level Four bar mass spectrogram of n-alkane.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
1. instrument and reagent
Instrument: Shimadzu Q2010 Ultra GC/GC/MS, is equipped with AOC-5000 Plus automatic sampler
Second eyeball, sodium chloride, analyzes pure.C8-C20 n-alkane standard items (Sigma-Aldrich, 1mL)
2, sample preparation
Take the fresh squeezing orange juice of 5 g in 10 mL headspace sampling bottles, add 2 g NaCl, seal.Adopt full-automatic solid-phase microextraction and full-automatic input mode to carry out enrichment and the parsing of sample.Online solid-phase microextraction condition is: extracting head is 85 μ m Polyacrylate self-action extracting head; Sample incubation temperature is 45
oc; Hatching balance 10 min; It is 12 mm that extracting head is inserted the sample bottle degree of depth; Extraction time is 20 min.
3, instrument condition
One dimension chromatographic column is non-polar column DB-1 15m × 0.25mm × 0.1 μ m;
Two dimension chromatographic column is polar column BPX-50 15m × 0.1mm × 0.1 μ m;
Carrier gas: He, flow velocity 1.0 ml/mL;
Sampling condition: injection port resolution temperature is 250
oc, resolves 5 min.Injector temperature is 250
oc;
Column oven heating schedule: initial temperature is 35
oc, keeps 1 min, then with 3
othe heating rate of C/min is warming up to 270
oc, keeps 5 min;
Modulator-demodular unit arranges: be 6 s modulation period; Cold spray air flow is 10 mL/min; The jet temperature of heat is 325
oc, the heat spray duration is 350 ms;
Mass spectrum condition: mass detector is level Four bar mass spectrum; Ion source temperature 230
oc; Interface temperature 280
oc; Solvent delay 3 min; Adopt full scan mode, sweep limit is 30 m/z-300 m/z, sweep frequency: 20000 Hz.
Mass spectrum condition: ion gun: EI ionization source, 250 DEG C of temperature, 280 DEG C of transmission line temperature, mass scanning scope 50-550amu, acquisition rate: 100 collection of illustrative plates per second, detector voltage: 1750V, ionization voltage :-70V.Data processing: Pegasus, library searching: NIST/PEST He
4, interpretation of result
(1) obtain the retention time of C8-C20 n-alkane under above-mentioned instrumental analysis condition, as shown in Figure 2.Figure mid point is the two-dimensional chromatogram of the n-alkane that obtains, is followed successively by from left to right C
8h
18,c
9h
20, C
10h
22, C
11h
24, C
12h
26, C
13h
28, C
14h
30, C
15h
32, C
16h
34, C
17h
36, C
18h
38, C
19h
40, C
20h
42.
(2) by online solid-phase microextraction adsorbs olefins class component, carry out the mass spectrophotometry of comprehensive two dimensional gas chromatography-level Four bar, the olefines component in fresh squeezing orange juice is detected.The retention index computing method that adopt GC image Verson 2.3 to carry, calculate the retention time index of all olefines components that detect, according to retention time exponential quantity, (as table 1), according to the retention time index C atom number of olefines component according to a preliminary estimate of compound.
(3) compose storehouse by NIST and treat qualitative olefines component and carry out library searching, detected components is carried out fuzzy qualitative, obtain multiple possible structural formula, then carry out finally qualitative in conjunction with C atom number.
(4), for the component that adopts comprehensive two dimensional gas chromatography to separate, adopt joint convolution technique to judge peak purity, to realizing the accurate quantitative analysis analysis to overlapping olefines component by selection ionic means.
Taking object in Fig. 11 as example, the retention time index calculating according to one dimension retention time is 1588, and the C atom number of this compound is 15, is then chosen as by forward five kinds of NIST library searching rank: α-Patchoulene (C
15h
24), Tricyclo[3.1.0.0 (2,4)] hexane (C
12h
20), 2-[1-(Adamantan-1-ylamino)-2,2,2-trifluoro-ethylidene]-malononitrile (C
15h
16f
3n
3), Isosorbide-5-Nitrae-Methanophthalazine (C
11h
18n
2), 1,3-Cyclopentadiene (C
11h
18), in conjunction with C atom number, finally determine that this compound is α-Patchoulene.
Claims (3)
1. the online solid-phase microextraction of application and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy detect a method for olefines component in orange juice, it is characterized in that, comprise the following steps:
1) sample, after the orthogonal separation of comprehensive two dimensional gas chromatography, is detected by level Four bar mass spectrum;
2) adopt the mode of retention time exponential sum NIST spectrum storehouse combination qualitative to olefines component;
3) by joint convolution technique, chromatogram peak purity is judged, carry out accurate quantitative analysis analysis for chromatogram overlap peak by different choice ion.
2. a kind of method of applying olefines component in online solid-phase microextraction and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy detection orange juice according to claim 1, is characterized in that, comprises the following steps:
1) the olefines component in orange juice adopts online solid-phase microextraction Extraction and enrichment
Take and be less than the fresh squeezing orange juice of 5 g in 10 mL headspace sampling bottles, add excessive NaCl(approximately 2 g), seal, adopt full-automatic solid-phase microextraction and full-automatic input mode to carry out the sorption and desorption of sample;
2) adopt comprehensive two dimensional gas chromatography-level Four bar Mass Spectrometer Method
Use comprehensive two dimensional gas chromatography-level Four bar mass spectrometer to detect olefines component: by Using Automated Solid Phase Microextraction adsorption and enrichment olefines component, being adsorbed in the mode that the determinand in extracting head analyses by pyrolysis at injection port enters in comprehensive two dimensional gas chromatography-level Four bar mass spectrometer, component to be measured is after one dimension chromatographic column separates, after modulation /demodulation, enter two-dimensional gas chromatography post and separate, olefines component detects by the mass spectrographic full scan of level Four bar;
3) adopt the mode of retention time exponential sum NIST spectrum storehouse combination qualitative to olefines component
A) data analysis adopts GC image version 2.3;
B) the n-alkane standard items of C8-C20, adopt gas sampling pattern, utilize comprehensive two dimensional gas chromatography-level Four bar mass spectrum to analyze, obtain the retention time of C8-C20 n-alkane in a peacekeeping two dimension, the retention time index of the n-alkane of artificial definition C8-C20, the n-alkane retention time Index Definition that is 8 as atom number is 800, by that analogy (C atom number × 100);
C) according to the retention time index of the retention time calculating target compound of olefines component;
D) when sample is in the time that EI ionization source ionizes, its mass spectrogram and NIST spectrum storehouse compare, and when similarity is greater than setting value, this material is automatically recognized;
E) carry out qualitative in conjunction with retention time exponential sum NIST spectrum library searching result to olefines component;
4) quantitative test of olefines component
A) directly record peak area for the good olefines component of degree of separation;
B) for chromatogram overlap peak, adopt joint convolution technique to judge peak purity, when judging what peak overlapped to form as various ingredients, survey by selecting ionic means to distinguish quantitative test to overlap peak.
3. a kind of method of applying olefines component in online solid-phase microextraction and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy detection orange juice according to claim 2, is characterized in that described step 2) middle comprehensive two dimensional gas chromatography condition:
One dimension chromatographic column is non-polar column DB-1 15m × 0.25mm × 0.1 μ m;
Two dimension chromatographic column is polar column BPX-50 15m × 0.1mm × 0.1 μ m;
Carrier gas: He, flow velocity 1.0 mL/min;
Sampling condition: injection port resolution temperature is 250
oc, resolves 5 min;
Injector temperature is 250
oc;
Column oven heating schedule: initial temperature is 35 ~ 40
oC, keep 1 ~ 2 min, then with 3 ~ 5
othe heating rate of C/min is warming up to 270 ~ 300
oc, keeps 5 ~ 8 min;
Modulator-demodular unit arranges: be 6 s modulation period; Cold spray air flow is 10 mL/min; The jet temperature of heat is 325
oc, the heat spray duration is 350 ms;
Mass spectrum condition: mass detector is level Four bar mass spectrum; Ion source temperature 230
oc; Interface temperature 280
oc; Solvent delay 3 ~ 4 min; Adopt full scan mode, sweep limit is 30 m/z-300 m/z, sweep frequency: 20000 Hz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410232628.4A CN104034836A (en) | 2014-05-28 | 2014-05-28 | Method for detecting olefin components in orange juice by applying on-line solid-phase microextraction method and comprehensive two-dimensional gas chromatography-quadrupole mass spectrography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410232628.4A CN104034836A (en) | 2014-05-28 | 2014-05-28 | Method for detecting olefin components in orange juice by applying on-line solid-phase microextraction method and comprehensive two-dimensional gas chromatography-quadrupole mass spectrography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104034836A true CN104034836A (en) | 2014-09-10 |
Family
ID=51465684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410232628.4A Pending CN104034836A (en) | 2014-05-28 | 2014-05-28 | Method for detecting olefin components in orange juice by applying on-line solid-phase microextraction method and comprehensive two-dimensional gas chromatography-quadrupole mass spectrography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104034836A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887923A (en) * | 2019-12-02 | 2020-03-17 | 太原理工大学 | Method for detecting nitrogen and sulfur compounds in tar by using full-two-dimensional gas chromatograph-mass spectrometer |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6494078B1 (en) * | 2001-06-25 | 2002-12-17 | Agilent Technologies, Inc. | Retention-time locked comprehensive multidimensional gas chromatography |
| CN101059484A (en) * | 2007-04-14 | 2007-10-24 | 粟学俐 | Use of comprehensive two-dimensional gas chromatography in flavored beer development |
| CN101680862A (en) * | 2006-10-25 | 2010-03-24 | 普拉德研究及开发股份有限公司 | Use GC * GC that hydrocarbon samples is carried out high accuracy contamination estimation |
| CN102914608A (en) * | 2012-11-12 | 2013-02-06 | 天津出入境检验检疫局动植物与食品检测中心 | Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer |
| JP2013068444A (en) * | 2011-09-21 | 2013-04-18 | Shimadzu Corp | Comprehensive two-dimensional chromatograph mass analysis data processing apparatus |
-
2014
- 2014-05-28 CN CN201410232628.4A patent/CN104034836A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6494078B1 (en) * | 2001-06-25 | 2002-12-17 | Agilent Technologies, Inc. | Retention-time locked comprehensive multidimensional gas chromatography |
| CN101680862A (en) * | 2006-10-25 | 2010-03-24 | 普拉德研究及开发股份有限公司 | Use GC * GC that hydrocarbon samples is carried out high accuracy contamination estimation |
| CN101059484A (en) * | 2007-04-14 | 2007-10-24 | 粟学俐 | Use of comprehensive two-dimensional gas chromatography in flavored beer development |
| JP2013068444A (en) * | 2011-09-21 | 2013-04-18 | Shimadzu Corp | Comprehensive two-dimensional chromatograph mass analysis data processing apparatus |
| CN102914608A (en) * | 2012-11-12 | 2013-02-06 | 天津出入境检验检疫局动植物与食品检测中心 | Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer |
Non-Patent Citations (2)
| Title |
|---|
| CARLA DA PORTO ET AL.: "Analyses of orange spirit flavour by direct-injection gas chromatography–mass spectrometry and headspace solid-phase microextraction/GC–MC", 《FLAVOUR AND FRAGRANCE JOURNAL》, vol. 18, 31 December 2003 (2003-12-31), pages 66 - 72 * |
| S´ıLVIA M. ROCHA ET AL.: "Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry of monoterpenoids as a powerful tool for grape origin traceability", 《JOURNAL OF CHROMATOGRAPHY A》, vol. 1161, 6 June 2007 (2007-06-06) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887923A (en) * | 2019-12-02 | 2020-03-17 | 太原理工大学 | Method for detecting nitrogen and sulfur compounds in tar by using full-two-dimensional gas chromatograph-mass spectrometer |
| CN110887923B (en) * | 2019-12-02 | 2022-02-08 | 太原理工大学 | Method for detecting nitrogen and sulfur compounds in tar by using full-two-dimensional gas chromatograph-mass spectrometer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Majchrzak et al. | PTR-MS and GC-MS as complementary techniques for analysis of volatiles: A tutorial review | |
| Nolvachai et al. | Multidimensional gas chromatography in food analysis | |
| Grimalt et al. | Review of analytical methods for the determination of pesticide residues in grapes | |
| Wu | Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry | |
| López et al. | Evaluation and validation of an accurate mass screening method for the analysis of pesticides in fruits and vegetables using liquid chromatography–quadrupole-time of flight–mass spectrometry with automated detection | |
| CN104849390B (en) | A kind of method of applying component in the qualitative white wine of comprehensive two dimensional gas chromatography-flight time mass spectrum coupling | |
| CN103995078B (en) | Apply the method for ester class component in online solid-phase microextraction and comprehensive two dimensional gas chromatography-level Four bar mass spectroscopy detection orange juice | |
| Qin et al. | Automated multi-plug filtration cleanup for liquid chromatographic–tandem mass spectrometric pesticide multi-residue analysis in representative crop commodities | |
| CN103983712B (en) | Apply the method for ketone component in online solid-phase microextraction and comprehensive two dimensional gas chromatography-level Four bar mass spectrography detection orange juice | |
| AU2019100393A4 (en) | Method for detecting alcohol components in orange juice through online-solid-phase micro-extraction and comprehensive two-dimensional gas chromatography/quadrupole mass spectrometer | |
| CN106290545B (en) | A kind of method and device of detection trace compound | |
| CN103105440A (en) | Method for identifying volatile flavor substance in bolete | |
| CN105806974A (en) | Detection method of aroma components of rubus biflorus fruits | |
| CN103823033A (en) | Analyzing and detecting method of flavor compound in white spirit | |
| CN104034820A (en) | Method for rapidly distinguishing brand of kirschwasser | |
| CN103162994A (en) | Ultra-low temperature extraction device and analysis method of smoke aroma components by using ultra-low temperature extraction device | |
| CN110596255A (en) | Method for detecting volatile components of tomatoes and products thereof | |
| CN104062306A (en) | Mass-spectrum rapid analysis method for pesticide residue in fruits and vegetables | |
| Donato et al. | Analysis of the carotenoid composition and stability in various overripe fruits by comprehensive two-dimensional liquid chromatography | |
| CN102706982A (en) | Method for analyzing constituents of white spirit | |
| CN104034836A (en) | Method for detecting olefin components in orange juice by applying on-line solid-phase microextraction method and comprehensive two-dimensional gas chromatography-quadrupole mass spectrography | |
| Wang et al. | Determination of multiclass pesticide residues in apple juice by gas chromatography–mass spectrometry with large‐volume injection | |
| AU2019100394A4 (en) | Method for detecting olefin components in orange juice through online-solid-phase micro-extraction and comprehensive two-dimensional gas chromatography/quadrupole mass spectrometer | |
| Teonata et al. | An Introduction to Different Types of Gas Chromatography | |
| CN103743849A (en) | Ion chromatography-high resolution mass spectrum hyphenation method for screening and authenticating multiple organic acids in dairy products synchronously and rapidly |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140910 |