CN102706982A - Method for analyzing constituents of white spirit - Google Patents
Method for analyzing constituents of white spirit Download PDFInfo
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- CN102706982A CN102706982A CN2012102201881A CN201210220188A CN102706982A CN 102706982 A CN102706982 A CN 102706982A CN 2012102201881 A CN2012102201881 A CN 2012102201881A CN 201210220188 A CN201210220188 A CN 201210220188A CN 102706982 A CN102706982 A CN 102706982A
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Abstract
The invention discloses a method for analyzing constituents of white spirit, which is capable of detecting more constituents. The method comprises the steps of: carrying out condition normalization on an SBSE (stir bar sorptive extraction) stir bar by a thermal desorption apparatus, then absorbing target matters in a white spirit sample by the SBSE puddler, transferring the SBSE stir bar to a desorption chamber of the thermal desorption apparatus, desorbing the absorbed target matters to a program heating sample inlet through the thermal desorption apparatus, providing the target matters in GC*GC-TOFMS (comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer) to separate and analyze via the program heating sample inlet, wherein the used SBSE stir bars respectively are the SBSE stir bar with a polydimethylsiloxane absorption layer and the SBSE stir bar with a polyethylene glycol modified organic silicon absorption layer. The result is accurate and reliable; the sensitivity is high, and the method can be used for analyzing the constituents of all white spirit, is particularly suitable for analysis of a micro-constituent of which the mass percentage is 0.01-0.1%, and also can be used for analysis of a trace constituent of which the mass percentage is smaller than 0.01%.
Description
Technical field
The present invention relates to liquor constituent analysis field, especially a kind of liquor component analyzing method.
Background technology
China's conventional solid-state fermentation liquor is the time-honored unique product of the Chinese nation, is one of the world's six big famous Spirit kinds, receives domestic and international vast drink person's praise deeply.Its selected multiple high-quality grain is raw material, adopts multiple microorganism to inoculate the system song naturally that unique brewage process has been given its unique flavour characteristic.
The trace flavor component that comprises One's name is legion in the liquor.Micro constitutent in China's conventional solid-state fermentation liquor is very abundant, from classification alcohols, ester class, acids, aldoketones, carbonyls, heterogeneous ring compound or the like is arranged, and some of them also have physiologically active.
In the last few years,, a large amount of work had been done in the analysis of fragrance matter in the Chinese conventional solid-state fermentation liquor, obtained significant achievement along with improving constantly of instrumental analysis level.Can detect through modern analytical techniques such as gas chromatography, gas-matter coupling, liquid chromatographies at present and reach over one hundred kind fragrance matter in the liquor.But because conventional solid-state fermentation liquor production process is unique, composition is abundant, and the analysis work of micro substance in the liquor is still failed all to accomplish, and also has many micro substances still to be in unknown state; Simultaneously, still study not deep enoughly to chromatographic resolution analytical technology, the sample extraction concentration technique of micro substance in the liquor, therefore, the micro substance in the further investigation liquor is still one of important topic of conventional solid-state fermentation liquor flavor research.
Stir Bar Sorptive Extraction technology (SBSE) is the abstraction technique that a kind of newly-developed gets up.The SBSE technology is that the glass capsulation bar magnet (SBSE stirring rod) that skin scribbles the stationary phase adsorbed layer is directly put into sample, utilize magnetic stirring apparatus to make it to contact and enriched sample in the method for compound.(SPME) compares with SPME; Stir Bar Sorptive Extraction technology (SBSE) the stationary phase that uses much bigger; Consumption is more than 50 times of SPME; Have than littler the comparing of SPME (water volume/PDMS phase volume), thereby make detection sensitivity increase by 100 to 1000 times, and have the higher recovery.
Thermal desorption appearance (TDU) is a kind of instrument with SBSE stirring rod Combined application.Put into the desorption chamber of TDU to the SBSE stirring rod, thereby TDU can heat the material desorption that is attracted on the SBSE stirring rod is fallen.The programmed temperature sampling mouth is called the CIS injection port again; It uses with TDU, and in the TDU heating, the temperature in the CIS injection port can drop to very low; The material that is upward got off by desorption from TDU so just is condensed and concentrates in the CIS injection port; The CIS injection port is rapidly heated then, material is pushed in the chromatographic column, thereby can carry out compartment analysis to material.
Thermal desorption appearance (TDU) and the SBSE stirring rod supporting with it are known at present has German GERSTEL company product; The CIS injection port is known at present has U.S. Agilent company to produce.
Comprehensive two dimensional gas chromatography (Comprehensive Two-dimensional Gas Chromatography; GC * GC) is the new method that occurs the beginning of the nineties, it be the separating mechanism difference and mutually independently two chromatographic columns be combined into comprehensive two dimensional gas chromatography with series system.Between these two chromatographic columns, a modulator is housed, plays freezing capture and transmit again.When analyzing, the component after each separates through first chromatographic column all is introduced into modulator, carries out delivering to second chromatographic column with the mode of intensification pulse again after the freezing focusing and further separates, and then get into detecting device and carry out analyzing and testing.Comprehensive two dimensional gas chromatography is compared with the one dimension chromatogram, have that resolution height, peak capacity are big, highly sensitive, analysis time advantage such as weak point, qualitative good reliability, very be fit to analyze as liquor, forms the complicated material system.
Time of-flight mass spectrometer (TOFMS) has all been compared remarkable advantages than common quadrupole mass spectrometer at aspects such as sensitivity, stability, ion scan usefulness, noise reduction capability, be at present unique can with the mass spectrometer of GC * GC well matched.
Comprehensive two dimensional gas chromatography-flight time mass spectrum that comprehensive two dimensional gas chromatography appearance and time of-flight mass spectrometer are arranged in pairs or groups mutually (GC * GC-TOFMS), can be described as at present the most powerful makings instrument of analytic function in the world.
Also stirring and adsorbing abstraction technique SBSE and GC * GC-TOFMS are not applied to the relevant report of liquor component analysis at present.
Summary of the invention
Detect the less deficiency of composition in order to overcome existing liquor component analyzing method, technical matters to be solved by this invention provides a kind of liquor component analyzing method that can detect more kinds of compositions.
The technical solution adopted for the present invention to solve the technical problems is: the liquor component analyzing method; With the target substance in the SBSE stirring rod absorption liquor sample; The SBSE stirring rod is transferred to the desorption chamber of thermal desorption appearance; With target substance desorption to the programmed temperature sampling mouth that is adsorbed, target substance gets into GC * GC-TOFMS via the programmed temperature sampling mouth and carries out compartment analysis through the thermal desorption appearance.
Further be before the SBSE stirring rod is dropped into the liquor sample, the SBSE stirring rod to be carried out the condition standardization with the thermal desorption appearance.
Described SBSE stirring rod normalization condition does, new SBSE stirring rod is placed in the empty thermal desorption glass tube, and be desorption 30 minutes in 240 ℃ the thermal desorption appearance at desorption temperature, helium gas flow is 50mL/min.
Further be that employed SBSE stirring rod is the SBSE stirring rod with dimethyl silicone polymer adsorbed layer.
The thermal desorption process of said SBSE stirring rod is: the SBSE stirring rod is transferred to the desorption chamber of 15 ℃ of initial temperatures, be warming up to 300 ℃ and kept 7 minutes; In the thermal desorption process; Carrier gas is brought target substance into and is cooled in-50 ℃ the programmed temperature sampling mouth; Target substance low temperature in the programmed temperature sampling mouth is assembled; After treating that the thermal desorption process is accomplished, the programmed temperature sampling mouth is warming up to 300 ℃ rapidly and target substance is sent into GC * GC-TOFMS carries out compartment analysis.
Corresponding with aforementioned schemes, the chromatographic condition of complete two-dimentional gas chromatography mass spectrometry: injector temperature: 250 ℃; Carrier gas: He; Main baking oven heating schedule: 45 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 4 ℃/min, be raised to 250 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 4 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.
Further be that employed SBSE stirring rod is the SBSE stirring rod with organosilicon adsorbed layer of polyglycol improvement.
The thermal desorption process of said SBSE stirring rod is: the SBSE stirring rod is transferred to the desorption chamber of 15 ℃ of initial temperatures, be warming up to 250 ℃ and kept 10 minutes; In the thermal desorption process; Carrier gas is brought target substance into and is cooled in-30 ℃ the programmed temperature sampling mouth; Target substance low temperature in the programmed temperature sampling mouth is assembled; After treating that the thermal desorption process is accomplished, the programmed temperature sampling mouth is warming up to 300 ℃ rapidly and target substance is sent into GC * GC-TOFMS carries out compartment analysis.
Corresponding with aforementioned schemes, the chromatographic condition of complete two-dimentional gas chromatography mass spectrometry: injector temperature: 250 ℃; Carrier gas: He; Main baking oven heating schedule: 40 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 3 ℃/min, be raised to 245 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 3 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.
Further be that employed SBSE stirring rod is respectively the SBSE stirring rod of SBSE stirring rod with dimethyl silicone polymer adsorbed layer and the organosilicon adsorbed layer with polyglycol improvement.
The invention has the beneficial effects as follows: SBSE stirring rod extraction does not need organic solvent, is a kind of environmentally friendly, easy abstraction technique, is highly suitable for the separation of trace organic substance in the fluid sample and concentrates; With SBSE mutually coupling be the thermal desorption appearance; It can unite use with gas chromatography well through the programmed temperature sampling mouth, and the material that SBSE is extracted into is sent in the gas chromatography and analyzed, and the result accurately and reliably; Highly sensitive; Can in liquor, detect over thousands of kind of micro constitutent,, can be used for analyzing the composition of various liquor considerably beyond used other analytical approachs detected material composition in liquor in the past; Be particularly suitable for mass percent wherein in 0.01～0.1% micro constitutent analysis, also can be used for the wherein analysis of the trace constituent of mass percent＜0.01%.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Liquor component analyzing method of the present invention is with the target substance in the SBSE stirring rod absorption liquor sample; The SBSE stirring rod is transferred to the desorption chamber of thermal desorption appearance; With target substance desorption to the programmed temperature sampling mouth that is adsorbed, target substance gets into GC * GC-TOFMS via the programmed temperature sampling mouth and carries out compartment analysis through the thermal desorption appearance.
Further be; Before the SBSE stirring rod is dropped into the liquor sample; With the thermal desorption appearance SBSE stirring rod is carried out the condition standardization, thus avoid as far as possible the SBSE stirring rod produce or the preservation process in maybe adsorbent to the influence of follow-up absorption and analytic process.
Roughly kind according to contained material in the liquor; After test, drawing the SBSE stirring rod normalization condition that is suitable for material absorption in the liquor does; New SBSE stirring rod is placed in the empty thermal desorption glass tube; At desorption temperature is desorption 30 minutes in 240 ℃ the thermal desorption appearance, and helium gas flow is 50mL/min.
After deliberation; Be suitable for liquor and analyze the SBSE stirring rod that employed SBSE stirring rod preferably has the dimethyl silicone polymer adsorbed layer; This stirring rod has good adsorption effect for nonpolar compound; And another kind of SBSE stirring rod with organosilicon adsorbed layer of polyglycol improvement, this absorption rod has the good adsorption effect for the polar material that has hydrogen bond functional group.
After deliberation, be suitable for said thermal desorption process and be: the SBSE stirring rod is transferred to the desorption chamber of 15 ℃ of initial temperatures, be warming up to 300 ℃ and kept 7 minutes with SBSE stirring rod of dimethyl silicone polymer adsorbed layer; In the thermal desorption process; Carrier gas is brought target substance into and is cooled in-50 ℃ the programmed temperature sampling mouth; Target substance low temperature in the programmed temperature sampling mouth is assembled; After treating that the thermal desorption process is accomplished, the programmed temperature sampling mouth is warming up to 300 ℃ rapidly and target substance is sent into GC * GC-TOFMS carries out compartment analysis.
Mainly adsorb apolar substance owing to have the SBSE stirring rod of dimethyl silicone polymer adsorbed layer, after deliberation, the chromatographic condition of complete two-dimentional gas chromatography mass spectrometry that adapts therewith is: injector temperature: 250 ℃; Carrier gas: He; Main baking oven heating schedule: 45 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 4 ℃/min, be raised to 250 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 4 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.
After deliberation, the thermal desorption process that is suitable for the SBSE stirring rod of said organosilicon adsorbed layer with polyglycol improvement is: the SBSE stirring rod is transferred to the desorption chamber of 15 ℃ of initial temperatures, be warming up to 250 ℃ and kept 10 minutes; In the thermal desorption process; Carrier gas is brought target substance into and is cooled in-30 ℃ the programmed temperature sampling mouth; Target substance low temperature in the programmed temperature sampling mouth is assembled; After treating that the thermal desorption process is accomplished, the programmed temperature sampling mouth is warming up to 300 ℃ rapidly and target substance is sent into GC * GC-TOFMS carries out compartment analysis.
Mainly adsorb the polar material that has hydrogen bond functional group owing to have the SBSE stirring rod of the organosilicon adsorbed layer of polyglycol improvement, after deliberation, the chromatographic condition of complete two-dimentional gas chromatography mass spectrometry that adapts therewith is: injector temperature: 250 ℃; Carrier gas: He; Main baking oven heating schedule: 40 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 3 ℃/min, be raised to 245 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 3 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.
For the liquor sample is carried out multianalysis; Best employed SBSE stirring rod is each one of the SBSE stirring rod of SBSE stirring rod with dimethyl silicone polymer adsorbed layer and the organosilicon adsorbed layer with polyglycol improvement, thereby can from the liquor sample, fully extract a greater variety of micro constitutents.Use above-mentioned method, in certain aromatic Chinese spirit, detect the microcomponent of kind surplus in the of 1800, detect the microcomponent about 1700 kinds in certain Maotai-flavor liquor, in certain fen-flavor type white spirit, detect the microcomponent about 1300 kinds.
Embodiment:
1, main agents and sample
Pure water (through Milli-Q Adavantage A10 ultrapure water system handles), certain aromatic Chinese spirit.
2, key instrument
GC * GC system is made up of Agilent6890 gas chromatograph and cold spray modulator; First chromatographic column of comprehensive two dimensional gas chromatography appearance: DB-FFAP (J&W Scientific, Agilent Technologies); The second chromatographic column DB-1701 (J&Wscientific, Agilent Technologies).Time of-flight mass spectrometer is the PegasusIV of U.S. Leco company.SBSE stirring rod: German GERSTEL company; TDU thermal desorption sampling device: German GERSTEL company.
3, concrete grammar
(1) new SBSE stirring rod is carried out the condition standardization, method is that the SBSE stirring rod is placed in the empty thermal desorption glass tube, is desorption 30 minutes in 240 ℃ the thermal desorption appearance at desorption temperature, and helium gas flow is 50mL/min.
(2) in 20ml headspace sampling bottle, add liquor sample 10mL, put into the SBSE stirring rod of (PDMS) coating that has dimethyl silicone polymer, with barrier film screw capping sealing top empty bottle mouth.Be placed on the head space bottle on the magnetic stirring apparatus, let the SBSE stirring rod stir 2 hours at the rotating speed lower magnetic force of 1000r/min.After absorption is accomplished, gently the SBSE stirring rod is taken out,, wipe the water droplet on surface again away with clean no cotton fiber cloth with a little pure water washing SBSE stirring rod surface with magnetism stick.
(3) take by weighing 10ml wine appearance and add in the head space bottle of 20ml, put into the SBSE stirring rod of organosilicon adsorbed layer then, with barrier film screw capping sealing top empty bottle mouth with polyglycol (PEG) improvement.Be placed on the head space bottle on the magnetic stirring apparatus, let the SBSE stirring rod stir 2 hours at the rotating speed lower magnetic force of 1000r/min.After absorption is accomplished, gently the SBSE stirring rod is taken out,, wipe the water droplet on surface again away with clean no cotton fiber cloth with a little pure water washing SBSE stirring rod surface with magnetism stick.
(4) the SBSE stirring rod that step (2) is obtained is transferred to the TDU desorption chamber of 15 ℃ of initial temperatures, is warming up to 300 ℃ and kept 7 minutes, and this is the thermal desorption process of target substance.Carrier gas is brought target substance among the CIS4 that is cooled to-50 ℃ in desorption process, and target substance low temperature in CIS4 is assembled, treat that the thermal desorption process is accomplished after, CIS4 is warming up to 300 ℃ rapidly and target substance is sent into GC * GC/TOFMS carries out compartment analysis.The chromatographic condition of complete two-dimentional gas chromatography mass spectrometry: injector temperature: 250 ℃; Carrier gas: He; Main baking oven temperature programme: 45 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 4 ℃/min, be raised to 250 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 4 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min.EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.Count the mass spectrometric data of scope 28-500 with 100 full spectrogram/frequency acquisition acquisition qualities of second, the gained data are advanced automatic processing through the workstation of Pegasus4D again, and qualitative used spectrogram storehouse is NIST/EPA/NIH Version2.0.
(5) the SBSE stirring rod that step (3) is obtained is transferred to the TDU desorption chamber of 15 ℃ of initial temperatures, is warming up to 250 ℃ and kept 10 minutes, and this is the thermal desorption process of target substance.Carrier gas is brought target substance among the CIS4 that is cooled to-30 ℃ in desorption process, and target substance low temperature in CIS4 is assembled, treat that the thermal desorption process is accomplished after, CIS4 is warming up to 300 ℃ rapidly and target substance is sent into GC * GC/TOFMS carries out compartment analysis.The chromatographic condition of complete two-dimentional gas chromatography mass spectrometry: injector temperature: 250 ℃; Carrier gas: He; Main baking oven temperature programme: 40 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 3 ℃/min, be raised to 245 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 3 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min.EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.Count the mass spectrometric data of scope 28-500 with 100 full spectrogram/frequency acquisition acquisition qualities of second, the gained data are advanced automatic processing through the workstation of Pegasus4D again, and qualitative used spectrogram storehouse is NIST/EPA/NIHVersion2.0.
(6) twice analysis result is comprehensive, remove wherein identical compound, finally obtain the analysis result of microcomponent in the liquor.
Use this technology; Testing result shows: contain 1870 kinds of components in the said liquor; And accurately qualitatively gone out 1227 kinds of micro constitutents wherein, also found the functional component of multiple beneficial, comprising Tetramethylpyrazine kind of pyrazine class material surplus interior ten in health.
Sample wine compositional classification sees the following form 1:
Table 1: sample wine compositional classification table
| Classes of compounds | Aldehydes | Ketone | Alcohols | Acids | The ester class | Other |
| Amount detection | 43 | 128 | 154 | 68 | 394 | 1083 |
Sample wine mainly detects material and sees the following form 2:
Table 2: sample wine mainly detects material
Claims (10)
1. liquor component analyzing method; It is characterized in that: with the target substance in the SBSE stirring rod absorption liquor sample; The SBSE stirring rod is transferred to the desorption chamber of thermal desorption appearance; With target substance desorption to the programmed temperature sampling mouth that is adsorbed, target substance gets into GC * GC-TOFMS via the programmed temperature sampling mouth and carries out compartment analysis through the thermal desorption appearance.
2. liquor component analyzing method as claimed in claim 1 is characterized in that: before the SBSE stirring rod is dropped into the liquor sample, with the thermal desorption appearance SBSE stirring rod is carried out the condition standardization.
3. liquor component analyzing method as claimed in claim 2; It is characterized in that: described SBSE stirring rod normalization condition does; New SBSE stirring rod is placed in the empty thermal desorption glass tube, is desorption 30 minutes in 240 ℃ the thermal desorption appearance at desorption temperature, and helium gas flow is 50mL/min.
4. like claim 1,2 or 3 described liquor component analyzing methods, it is characterized in that: employed SBSE stirring rod is the SBSE stirring rod with dimethyl silicone polymer adsorbed layer.
5. liquor component analyzing method as claimed in claim 4 is characterized in that: the thermal desorption process of said SBSE stirring rod is: the SBSE stirring rod is transferred to the desorption chamber of 15 ℃ of initial temperatures, be warming up to 300 ℃ and kept 7 minutes; In the thermal desorption process; Carrier gas is brought target substance into and is cooled in-50 ℃ the programmed temperature sampling mouth; Target substance low temperature in the programmed temperature sampling mouth is assembled; After treating that the thermal desorption process is accomplished, the programmed temperature sampling mouth is warming up to 300 ℃ rapidly and target substance is sent into GC * GC-TOFMS carries out compartment analysis.
6. liquor component analyzing method as claimed in claim 5 is characterized in that: the chromatographic condition of complete two-dimentional gas chromatography mass spectrometry: injector temperature: 250 ℃; Carrier gas: He; Main baking oven heating schedule: 45 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 4 ℃/min, be raised to 250 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 4 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.
7. like claim 1,2 or 3 described liquor component analyzing methods, it is characterized in that: employed SBSE stirring rod is the SBSE stirring rod with organosilicon adsorbed layer of polyglycol improvement.
8. liquor component analyzing method as claimed in claim 7 is characterized in that: the thermal desorption process of said SBSE stirring rod is: the SBSE stirring rod is transferred to the desorption chamber of 15 ℃ of initial temperatures, be warming up to 250 ℃ and kept 10 minutes; In the thermal desorption process; Carrier gas is brought target substance into and is cooled in-30 ℃ the programmed temperature sampling mouth; Target substance low temperature in the programmed temperature sampling mouth is assembled; After treating that the thermal desorption process is accomplished, the programmed temperature sampling mouth is warming up to 300 ℃ rapidly and target substance is sent into GC * GC-TOFMS carries out compartment analysis.
9. liquor component analyzing method as claimed in claim 8 is characterized in that: the chromatographic condition of complete two-dimentional gas chromatography mass spectrometry: injector temperature: 250 ℃; Carrier gas: He; Main baking oven heating schedule: 40 ℃ of initial temperature, keep 0.5min, be raised to 70 ℃ with 3 ℃/min, be raised to 245 ℃ with 5 ℃/min again, keep 25min; The second baking oven heating schedule: 60 ℃ of initial temperature, keep 0.5min, be raised to 90 ℃ with 3 ℃/min, be raised to 255 ℃ with 5 ℃/min again, keep 40min; EI ion source temperature: 200 ℃; Ionizing energy 70eV; Detector voltage: 1.57kV; Transmission line temperature: 260 ℃.
10. like claim 1,2 or 3 described liquor component analyzing methods, it is characterized in that: employed SBSE stirring rod is respectively the SBSE stirring rod of SBSE stirring rod with dimethyl silicone polymer adsorbed layer and the organosilicon adsorbed layer with polyglycol improvement.
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| CN103293141A (en) * | 2013-03-25 | 2013-09-11 | 江苏省质量安全工程研究院 | A liquor vintage recognition method based on a fusion technology of ion mobility spectrometry/ mass spectrometry/ Raman spectroscopy |
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| CN103969391A (en) * | 2014-05-23 | 2014-08-06 | 江南大学 | Method for determining volatile components in millet wine |
| CN110115991A (en) * | 2018-02-06 | 2019-08-13 | 爱普香料集团股份有限公司 | A kind of preparation and application method of GC/MS joint thermal desorption Solid Phase Extraction stick |
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| CN110554113A (en) * | 2019-09-12 | 2019-12-10 | 云南中烟工业有限责任公司 | method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS |
| CN110554113B (en) * | 2019-09-12 | 2022-04-01 | 云南中烟工业有限责任公司 | Method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS |
| CN114199986A (en) * | 2021-12-10 | 2022-03-18 | 河南牧业经济学院 | Method for simultaneously determining 3 aldehyde compounds in beer |
| CN114199986B (en) * | 2021-12-10 | 2024-05-07 | 河南牧业经济学院 | Method for simultaneously measuring 3 aldehyde compounds in beer |
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Application publication date: 20121003 |