CN103018370A - Method for judging important flavor substance of liquor - Google Patents
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Abstract
The invention discloses a method for judging an improtant flavor substance of liquor. The method comprises the steps of diluting a liquor sample to be detected with deionized water till the final alcohol content is 12-14%vol, conducting headspace solid-phase microextraction on a flavor compound in the enriched sample, measuring with comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry, conducting fragrance smelling judgment with a smell detector synchronously to qualitatively analyze the major flavor substance of the liquor, and quantitatively analyzing the confirmed important flavor substance of the liquor by a standard curve internal standard method. The method for quickly and comprehensively analyzing key fragrance, characteristic fragrance and important fragrance compounds in the flavor compound of the liquor is established, a technical system integrating a qualitative method, a quantitative method and sensation for the flavor compound of the liquor, and an evaluation system are established, and an effective tool is further provided for analyzing micro constituents of the liquor.
Description
Technical field
The invention belongs to the local flavor analysis technical field of liquor, be a kind of method of identifying the important flavor substance of liquor, be specifically related to headspace solid-phase microextraction and comprehensive two dimensional gas chromatography-flight time mass spectrum qualitative-and-quantitative method and sense of smell and hear the fragrant technical system of identifying the sensation combination.
Background technology
China white wine has determined that because of technique singularity its micro constitutent is very abundant.So far, in the China white wine qualitative detection to micro-flavor components broken through 1000 kinds, wherein can use more than 900 kinds that have that direct insertion technique and solid phase micro-extraction technique carry out qualitative, quantitative, but the content of nearly 100 kinds of materials is arranged at μ g or ng even the lower order of magnitude, these components also have a distinguishing feature, it is inner to be hidden in exactly the larger component peaks of liquor content, can't be detected by one dimension chromatogram or common gas chromatography mass spectrometry instrument, these compositions are the real important aroma compounds of China white wine, and they play vital effect to liquor style and liquor typical case and Style evolution.Therefore, set up a cover and analyze fast the method for crucial fragrance, characteristic perfume and important volatile compound in the aroma compound of liquor comprehensively, set up the qualitative-and-quantitative method of liquor flavor compound and the technical system of sensation combination, and appraisement system seems very necessary.
Headspace solid-phase microextraction (SPME) technology has and need not just effective component in the enriched sample of easily extraction, and have highly sensitive, detection limit is low, the characteristics such as simple to operate, quick; (GC * GC-TOFMS) other gas chromatography mass spectrometries have high sensitivity and high separation property to comprehensive two dimensional gas chromatography-flight time mass spectrum relatively, are particularly suitable for separating extremely complicated architectural study.Olfactometry device (ODP2) is conducive to hear the fragrant important aroma compound of identifying by sense of smell, therefore uses the SPME method, and GC * GC-TOFMS can be good at well estimating the important flavor substance of liquor in conjunction with ODP2.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method of identifying the important flavor substance of liquor, set up the qualitative-and-quantitative method of liquor flavor compound and the technical system of sensation combination, can analyze fast crucial fragrance, characteristic perfume and important volatile compound in the aroma compound of liquor comprehensively, the effective tool of Mysterious Veil of the micro constitutent of an analysis liquor is provided.
The present invention is achieved through the following technical solutions:
A kind of method of identifying the important flavor substance of liquor, with deionized water wine sample to be measured is diluted to final alcohol content 12-14%vol first, then use headspace solid-phase microextraction enriched sample flavor compound, use again comprehensive two dimensional gas chromatography-flight time mass spectrum coupling to measure, carry out fragrant evaluation of sense of smell news in conjunction with the olfactometry device synchronously the important flavor substance of liquor is carried out qualitative analysis, then by the typical curve internal standard method the important flavor substance of confirmed liquor is carried out quantitative test.
Concrete steps are as follows:
(1) described headspace solid-phase microextraction: wine sample 5 mL that draw after diluting put into 15 mL head space bottles, and add 2 g NaCl, screw bottle cap, place water-bath in 50 ℃ of constant temperature, in the head space bottle, insert simultaneously 50 μ m/30 μ m CAR/DVB/PDMS (2 cm) extracting head, balance 40 min;
(2) comprehensive two dimensional gas chromatography-flight time mass spectrum coupling: extract and extracting head is taken out after complete, insert the gas chromatographic sample introduction mouth, 250 ℃ of thermal desorption 5 min; Chromatographic column adopting GC * GC column system, first post 30m * 0.25mm * 0.25m, Rxi-17 (midpolarity phase; Crossbond 50%diphenyl/50%dimethylpolysiloxane), second post 1.2m * 0.1mm * 0.1 μ m, Rtx-5 (Crossbond 5%Diphenyl/95%dimethylpolysiloxane), two root chromatogram columns connect with series system by the capillary column connector, 280 ℃ of injector temperatures, sample size 1 μ L, constant voltage 600kPa before the post, split ratio 1:50, modulation period 4s, hot gas duration 1.6s, cold air duration 2.4s, carrier gas is He (purity 99.9995%); Heating schedule is during detection: 40 ℃ of the first column oven initial temperature, kept 2 minutes, and be raised to 210 ℃ with 6 ℃/min, keep 5min, 65 ℃ of the second column oven initial temperature kept 2 minutes, were raised to 220 ℃ with 6 ℃/min, keep 5min, solvent delay 180s, 10 ℃ of modulation compensated temperature, cooling medium is liquid nitrogen, hot modulator is pressurized air, and cold modulator is N
2(purity 99.9995%);
Flight time mass spectrum system condition: frequency acquisition 200 frames/s, acquisition quality scope 35～500amu, 250 ℃ of transmission line temperature, smoothly spectrogram is required counts 6, peak width 6,220 ℃ of EI ion source temperatures, Ion source pressure 70eV, detector voltage 1500V, data are processed and to be used the Pegasus4D workstation, obtain the comprehensive two dimensional gas chromatography of tested liquor wine sample-flight time mass spectrum separation graph;
(3) the fragrant evaluation heard in sense of smell: half of comprehensive two dimensional gas chromatography post flow enters the olfactometry device, six through hearing fragrant training above specialties half a year personnel judge of wine (three male three woman that sample wine, 30 years old mean age, two of the judging panels of country, economize two of judging panels, two of the judging panels of factory) carry out the Wen Xiang analysis, each member all has the liquor of being familiar with odor characteristics, evaluation to fragrance is distinguished with 16 little grades of 5 large grades, divides assignment according to the fragrance of fragrance is strong and weak with typicalness.Grade is that 0 expression does not have fragrance, 1-5 to represent that aroma strength is faint, and 6-10 represents that aroma strength is medium, and 11-15 represents that aroma strength is stronger, and 16 expression aroma strengths are the strongest.The typicalness with fragrance faint to aroma strength, that aroma strength is medium, aroma strength is stronger is distinguished assignment.For example aroma strength is faint, and not having the assignment of typicalness is 1, and the assignment that slightly is typical is 2, and the assignment that is typical is 3, and the assignment of medium typicalness is 4, and the assignment of stronger typicalness is 5., aroma strength medium for aroma strength carries out assignment according to same method more by force.Everyone repeats to hear fragrant 3 times every component, as long as the aroma strength that has any three people among six people to describe something is for three times 0, looking so this material aroma strength is 0, averages as final aroma strength value, obtains the final aroma strength value table of arranging;
(4) to the important flavor substance qualitative analysis of liquor: hear the fragrant final aroma strength value that the identifies table of arranging according to sense of smell, in conjunction with comprehensive two dimensional gas chromatography-important flavor substance of flight time mass spectrum separating spectrum affirmation liquor;
(5) the important aroma compound of confirmed liquor is carried out quantitative test: take the ratio of confirmed important aroma compound standard items and the peak area at internal standard compound characteristic ion peak as horizontal ordinate, confirmed important aroma compound standard items are ordinate with the ratio of internal standard compound concentration, the Criterion curve comes quantitatively by calibration curve method; Concrete steps are,
The preparation of former mixed standard solution: the standard items that accurately take by weighing respectively the important aroma compound of 0.1g, be dissolved in respectively in the 10mL chromatographic grade ethanol, as single mark storing solution, single mark storing solution of important aroma compound is respectively drawn 5-500 μ L put into volumetric flask, be settled to 50mL with the 12-14%vol ethanolic solution, as former mixed standard solution;
The foundation of typical curve: a series of concentration that the production standard Curves is used are that the ethanolic solution with 12-14%vol progressively dilutes former mixed standard solution and gets, obtain altogether the former mixed standard solution of 12 concentration gradients, the former mixed standard solution of each concentration gradient that accurate absorption 5mL prepares places respectively 15mL head space bottle, add respectively 10 μ L inner mark solutions, and add 2 g NaCl, screw bottle cap, successively the mixed standard solution of each concentration gradient carried out headspace solid-phase microextraction, take the ratio of the standard items of important aroma compound and the peak area at internal standard compound characteristic ion peak as horizontal ordinate, the standard items of important aroma compound are ordinate drawing standard curve with the ratio of internal standard compound concentration;
Important aroma compound is measured in the wine sample: wine sample alcoholic strength to be measured is diluted to 12-14%vol, add mark in the 10 μ L, use headspace solid-phase microextraction, comprehensive two dimensional gas chromatography-flight time mass spectrum carries out qualitative and quantitative analysis, important aroma compound content in the tested wine sample of reference standards curve determination;
Interior mark: take 2 – acetylpyridine as interior mark, quantitatively be limited to 0.05 μ g/L.
Beneficial effect of the present invention:
The present invention adopts headspace solid-phase microextraction-comprehensive two dimensional gas chromatography flight time mass spectrum to join olfactometry device coupling technique, sets up the authentication method of the important aroma compound of a cover liquor.(GC * GC) separates, (TOF) is qualitative for flight time mass spectrum by comprehensive two dimensional gas chromatography, identify odor characteristics in conjunction with olfactometry device (ODP), seek a collection of representative important aroma compound, effective tool of Mysterious Veil of the micro constitutent of having analyzed liquor further is provided.Set up a method of overlapping crucial fragrance, characteristic perfume and important volatile compound in the aroma compound of comprehensively analyzing fast liquor, set up the qualitative-and-quantitative method and the technical system of feeling combination of liquor flavor compound, and appraisement system.
Description of drawings
Fig. 1 be fragrant (1#) the important local flavor standard substance of sesame and in be marked on comprehensive two dimensional gas chromatography-flight time mass spectrum separation graph
Fig. 2 is the final aroma strength value of fragrant (1#) the important flavor substance of the sesame qualitative analysis sheet of table in conjunction with comprehensive two dimensional gas chromatography-flight time mass spectrum separation graph of arranging
Fig. 3 is important aroma compound content in the sesame cordiale, the recovery and precision quantitative test table
Wherein: 1-pyridine among Fig. 1; 2-thiazole; 3-methyl thiobutyrate; 4-3-methylthiopropionaldehyde; 5-methylmercaptan ethyl acetoacetic ester; 6-3 methylthiol propyl alcohol; 7-2-acetylpyridine (internal standard compound); 8-3-(methyl sulfo-) propionic acid ethyl ester; 9-benzothiazole.
Embodiment
To help to understand the present invention by following example, but not limit content of the present invention:
70%vol sesame-flavor wine sample (1#) is diluted to final alcohol content 12%vol with deionized water, (1) headspace solid-phase microextraction: draw 5ml wine sample as in the 10ml head space bottle, add 2gNaCl, screw bottle cap, place water-bath in 50 ℃ of constant temperature, in the head space bottle, insert simultaneously 50 μ m/30 μ m CAR/DVB/PDMS (2 cm) extracting head, balance 40 min.
(2) comprehensive two dimensional gas chromatography-flight time mass spectrum coupling: extract and extracting head is taken out after complete, insert the gas chromatographic sample introduction mouth, 250 ℃ of thermal desorption 5 min;
GC * GC column system: first post 30m * 0.25mm * 0.25m, Rxi-17 (midpolarityphase; Crossbond 50%diphenyl/50%dimethylpolysiloxane), second post 1.2m * 0.1mm * 0.1 μ m, Rtx-5 (Crossbond 5%Diphenyl/95%dimethylpolysiloxane), two root chromatogram columns connect with series system by the capillary column connector, 280 ℃ of injector temperatures, sample size 1 μ L, constant voltage 600kPa before the post, split ratio 1:50, modulation period 4s, hot gas duration 1.6s, cold air duration 2.4s, carrier gas is He (purity 99.9995%); Heating schedule is during detection: 40 ℃ of the first column oven initial temperature, kept 2 minutes, and be raised to 210 ℃ with 6 ℃/min, keep 5min, 65 ℃ of the second column oven initial temperature kept 2 minutes, were raised to 220 ℃ with 6 ℃/min, keep 5min, solvent delay 180s, 10 ℃ of modulation compensated temperature, cooling medium is liquid nitrogen, hot modulator is pressurized air, and cold modulator is N
2(purity 99.9995%);
Flight time mass spectrum system: frequency acquisition 200 frames/s, acquisition quality scope 35～500amu, 250 ℃ of transmission line temperature, smoothly spectrogram is required counts 6, peak width 6,220 ℃ of EI ion source temperatures, Ion source pressure 70eV, detector voltage 1500V, data are processed and to be used the egasus4D workstation, obtain the comprehensive two dimensional gas chromatography of tested liquor wine sample-flight time mass spectrum separation graph;
(3) the fragrant evaluation heard in sense of smell: half of comprehensive two dimensional gas chromatography post flow enters the olfactometry device, six through hearing fragrant training above specialties half a year personnel judge of wine (three male three woman that sample wine, 30 years old mean age, two of the judging panels of country, economize two of judging panels, two of the judging panels of factory) carry out the Wen Xiang analysis, each member all has the liquor of being familiar with odor characteristics, evaluation to fragrance is distinguished with 16 little grades of 5 large grades, divides assignment according to the fragrance of fragrance is strong and weak with typicalness.Grade is that 0 expression does not have fragrance, 1-5 to represent that aroma strength is faint, and 6-10 represents that aroma strength is medium, and 11-15 represents that aroma strength is stronger, and 16 expression aroma strengths are the strongest.The typicalness with fragrance faint to aroma strength, that aroma strength is medium, aroma strength is stronger is distinguished assignment.For example aroma strength is faint, and not having the assignment of typicalness is 1, and the assignment that slightly is typical is 2, and the assignment that is typical is 3, and the assignment of medium typicalness is 4, and the assignment of stronger typicalness is 5., aroma strength medium for aroma strength carries out assignment according to same method more by force.Everyone repeats to hear fragrant 3 times every component, as long as the aroma strength that has any three people among six people to describe something is for three times 0, looking so this material aroma strength is 0, averages as final aroma strength value, and the final aroma strength value table of arranging is determined in experiment repeatedly;
(4) to the important flavor substance qualitative analysis of liquor: hear the fragrant final aroma strength value that the identifies table of arranging according to sense of smell, in conjunction with comprehensive two dimensional gas chromatography-important flavor substance of flight time mass spectrum separating spectrum affirmation liquor;
(5) the important aroma compound of confirmed liquor is carried out quantitative test: take the ratio of confirmed important aroma compound standard items and the peak area at internal standard compound characteristic ion peak as horizontal ordinate, confirmed important aroma compound standard items are ordinate with the ratio of internal standard compound concentration, the Criterion curve comes quantitatively by calibration curve method; Concrete steps are,
The preparation of former mixed standard solution: the standard items that accurately take by weighing respectively the important aroma compound of 0.1g, be dissolved in respectively in the 10mL chromatographic grade ethanol, as single mark storing solution, single mark storing solution of important aroma compound is respectively drawn 5-500 μ L put into volumetric flask, be settled to 50mL with the 12-14%vol ethanolic solution, as former mixed standard solution; The foundation of typical curve: a series of concentration that the production standard Curves is used are that the ethanolic solution with 12-14%vol progressively dilutes former mixed standard solution and gets, obtain altogether the former mixed standard solution of 12 concentration gradients, the former mixed standard solution of each concentration gradient that accurate absorption 5mL prepares places respectively 15mL head space bottle, add respectively 10 μ L inner mark solutions, and add 2 g NaCl, screw bottle cap, successively the mixed standard solution of each concentration gradient carried out headspace solid-phase microextraction, take the ratio of the standard items of important aroma compound and the peak area at internal standard compound characteristic ion peak as horizontal ordinate, the standard items of important aroma compound are ordinate drawing standard curve with the ratio of internal standard compound concentration;
Important aroma compound is measured in the wine sample: certain sesame-flavor wine sample (1#) alcoholic strength is diluted to 12-14%vol, add mark in the 10 μ L, use headspace solid-phase microextraction, comprehensive two dimensional gas chromatography-flight time mass spectrum carries out qualitative and quantitative analysis, important aroma compound content in the tested wine sample of reference standards curve determination;
Interior mark: take 2 – acetylpyridine as interior mark, quantitatively be limited to 0.05 μ g/L.
60%vol sesame-flavor wine sample (2#) is identified that all the other are such as embodiment 1.
Claims (6)
1. method of identifying the important flavor substance of liquor, it is characterized in that: with deionized water wine sample to be measured is diluted to final alcohol content 12-14%vol first, then use headspace solid-phase microextraction enriched sample flavor compound, use again comprehensive two dimensional gas chromatography-flight time mass spectrum coupling to measure, carry out fragrant evaluation of sense of smell news in conjunction with the olfactometry device synchronously the important flavor substance of liquor is carried out qualitative analysis, then by the typical curve internal standard method the important flavor substance of confirmed liquor is carried out quantitative test.
2. method according to claim 1, it is characterized in that: described headspace solid-phase microextraction: wine sample 5 mL that draw after diluting put into 15 mL head space bottles, and add 2 g NaCl, screw bottle cap, place water-bath in 50 ℃ of constant temperature, in the head space bottle, insert simultaneously 50 μ m/30 μ m CAR/DVB/PDMS (2 cm) extracting head, balance 40 min.
3. method according to claim 2, it is characterized in that: described comprehensive two dimensional gas chromatography-flight time mass spectrum coupling: extract and extracting head is taken out after complete, insert the gas chromatographic sample introduction mouth, 250 ℃ of thermal desorption 5 min, chromatographic column adopting GC * GC column system, first post 30m * 0.25mm * 0.25m, second post 1.2m * 0.1mm * 0.1 μ m, two root chromatogram columns connect with series system by the capillary column connector, 280 ℃ of injector temperatures, constant voltage 600kPa before the sample size 1 μ L, post, split ratio 1:50, modulation period 4s, hot gas duration 1.6s, cold air duration 2.4s, carrier gas is He; Heating schedule is during detection: 40 ℃ of the first column oven initial temperature, kept 2 minutes, and be raised to 210 ℃ with 6 ℃/min, keep 5min, 65 ℃ of the second column oven initial temperature kept 2 minutes, were raised to 220 ℃ with 6 ℃/min, keep 5min, solvent delay 180s, 10 ℃ of modulation compensated temperature, cooling medium is liquid nitrogen, hot modulator is pressurized air, and cold modulator is N
2Flight time mass spectrum system condition: frequency acquisition 200 frames/s, acquisition quality scope 35～500amu, 250 ℃ of transmission line temperature, smoothly spectrogram is required counts 6, peak width 6,220 ℃ of EI ion source temperatures, Ion source pressure 70eV, detector voltage 1500V, data are processed and to be used the Pegasus4D workstation, obtain the comprehensive two dimensional gas chromatography of tested liquor wine sample-flight time mass spectrum separation graph.
4. method according to claim 3, it is characterized in that: the fragrant evaluation heard in described sense of smell: half of comprehensive two dimensional gas chromatography post flow enters the olfactometry device, the specialty personnel of sampling wine carry out Wen Xiang and analyze, evaluation to fragrance is distinguished with 16 little grades of 5 large grades, divide assignment according to fragrance is strong and weak with typicalness, make the final aroma strength value table of arranging.
5. method according to claim 4, it is characterized in that: described to the important flavor substance qualitative analysis of liquor: hear the fragrant final aroma strength value that the identifies table of arranging according to sense of smell, in conjunction with comprehensive two dimensional gas chromatography-important flavor substance of flight time mass spectrum separating spectrum affirmation liquor.
6. method according to claim 5, it is characterized in that: described the important aroma compound of confirmed liquor is carried out quantitative test: take the ratio of confirmed important aroma compound standard items and the peak area at internal standard compound characteristic ion peak as horizontal ordinate, confirmed important aroma compound standard items are ordinate with the ratio of internal standard compound concentration, the Criterion curve comes quantitatively by calibration curve method; Concrete steps are,
The preparation of former mixed standard solution: the standard items that accurately take by weighing respectively the important aroma compound of 0.1g, be dissolved in respectively in the 10mL chromatographic grade ethanol, as single mark storing solution, single mark storing solution of important aroma compound is respectively drawn 5-500 μ L put into volumetric flask, be settled to 50mL with the 12-14%vol ethanolic solution, as former mixed standard solution;
The foundation of typical curve: a series of concentration that the production standard Curves is used are that the ethanolic solution with 12-14% progressively dilutes former mixed standard solution and gets, obtain altogether the former mixed standard solution of 12 concentration gradients, the former mixed standard solution of each concentration gradient that accurate absorption 5mL prepares places respectively 15mL head space bottle, add respectively 10 μ L inner mark solutions, and add 2 g NaCl, screw bottle cap, successively the mixed standard solution of each concentration gradient carried out headspace solid-phase microextraction, take the ratio of the standard items of important aroma compound and the peak area at internal standard compound characteristic ion peak as horizontal ordinate, the standard items of important aroma compound are ordinate drawing standard curve with the ratio of internal standard compound concentration;
Important aroma compound is measured in the wine sample: wine sample alcoholic strength to be measured is diluted to 12-14%vol, add mark in the 10 μ L, use headspace solid-phase microextraction, comprehensive two dimensional gas chromatography-flight time mass spectrum carries out qualitative and quantitative analysis, important aroma compound content in the tested wine sample of reference standards curve determination;
Interior mark: take 2 – acetylpyridine as interior mark, quantitatively be limited to 0.05 μ g/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627599A (en) * | 2013-11-12 | 2014-03-12 | 中南大学 | Method for blending high-grade white spirit based on modern analysis technology |
| CN103823033A (en) * | 2014-03-24 | 2014-05-28 | 宜宾五粮液股份有限公司 | Analyzing and detecting method of flavor compound in white spirit |
| CN103869009A (en) * | 2014-01-22 | 2014-06-18 | 深圳市检验检疫科学研究院 | Method for determining main aroma components of wine |
| CN103969391A (en) * | 2014-05-23 | 2014-08-06 | 江南大学 | Method for determining volatile components in millet wine |
| CN104237435A (en) * | 2014-09-03 | 2014-12-24 | 上海应用技术学院 | Method for rapidly analyzing aroma components of distilled spirit |
| CN104849390A (en) * | 2015-05-29 | 2015-08-19 | 安徽古井贡酒股份有限公司 | Method for determining chemical composition in white spirit by adopting comprehensive two-dimensional gas chromatography-time of flight mass spectrometry |
| CN106018649A (en) * | 2016-07-14 | 2016-10-12 | 上海应用技术学院 | Identification method of nitrogen-containing compounds in Maotai |
| CN106018650A (en) * | 2016-07-14 | 2016-10-12 | 上海应用技术学院 | Method for identifying nitrogen-containing compound in kaoliang spirit |
| CN106124681A (en) * | 2016-07-14 | 2016-11-16 | 上海应用技术学院 | The authentication method of nitrogen-containing compound in a kind of Guo Jiao 1573 （The First Cellar in China） wine |
| CN106198804A (en) * | 2016-07-14 | 2016-12-07 | 上海应用技术学院 | The authentication method of nitrogen-containing compound in a kind of cherry wine |
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| CN106770707A (en) * | 2016-11-15 | 2017-05-31 | 国家烟草质量监督检验中心 | The screening method of volatile organic matter in a kind of quick-fried pearl of cigarette filter |
| CN107328876A (en) * | 2017-06-29 | 2017-11-07 | 安徽瑞思威尔科技有限公司 | A kind of method of volatile sulfur compounds in economic Quantitative detection white wine |
| CN107462624A (en) * | 2017-06-30 | 2017-12-12 | 江苏大学 | The rapid assay methods of main ester type compound content in a kind of white wine base liquor |
| CN108181390A (en) * | 2017-12-21 | 2018-06-19 | 北京工商大学 | The quantitative detecting method of sulfur-containing compound in a kind of white wine |
| CN109374759A (en) * | 2018-09-12 | 2019-02-22 | 北京工商大学 | A kind of method for concentration based on white wine liquid-liquid extraction |
| CN109959734A (en) * | 2019-03-21 | 2019-07-02 | 湖北工业大学 | The detection method of aroma compound in a kind of mixed-flavouring liquor |
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| CN113917061A (en) * | 2021-10-22 | 2022-01-11 | 贵州大学 | Detection and identification method for volatile substances of Maotai-flavor base liquor |
| CN113933428A (en) * | 2021-07-29 | 2022-01-14 | 杨晓军 | Quantitative analysis method for flavor substances in soy sauce flavor type round base liquor |
| WO2022016683A1 (en) * | 2020-07-20 | 2022-01-27 | 中山大学 | Laser ionization system for combined use of solid-phase microextraction and time of flight mass spectrometry |
| CN114062556A (en) * | 2021-11-19 | 2022-02-18 | 泸州老窖集团有限责任公司 | Carbon isotope composition detection method for white spirit flavor substances |
| CN114384169A (en) * | 2021-12-14 | 2022-04-22 | 贵州茅台酒股份有限公司 | Method for rapidly analyzing volatile flavor substances in white spirit based on large-volume sample injection static headspace gas chromatograph-mass spectrometer |
-
2012
- 2012-12-21 CN CN2012105591475A patent/CN103018370A/en active Pending
Non-Patent Citations (7)
| Title |
|---|
| 丁云连等: "老白干香型白酒香气成分分析", 《酿酒》 * |
| 季克良等: "全二维气相色谱/飞行时间质谱用于白酒微量成分的分析", 《酿酒科技》 * |
| 张艳红等: "顶空固相微萃取与气相色谱-火焰热离子检测器联用测定白酒中吡嗪类化合物", 《分析试验室》 * |
| 柳军: "口子窖和剑南春白酒香气物质研究", 《江南大学硕士学位论文》 * |
| 柳军等: "应用GC一0分析比较兼香型和浓香型白酒中的香气化合物", 《酿酒》 * |
| 胡风艳等: "应用DI-SPME和GC-MS分析白酒香气成分（上）", 《酿酒》 * |
| 鹿洪亮等: "全二维气相色谱-飞行时间质谱法测定烟草的中性化学成分", 《色谱》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627599A (en) * | 2013-11-12 | 2014-03-12 | 中南大学 | Method for blending high-grade white spirit based on modern analysis technology |
| CN103627599B (en) * | 2013-11-12 | 2015-09-30 | 中南大学 | A kind of method based on modern analytical technique allotment High Grade Liquor |
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| CN103823033B (en) * | 2014-03-24 | 2015-11-11 | 宜宾五粮液股份有限公司 | A kind of analyzing detecting method of white wine flavor compound |
| CN103823033A (en) * | 2014-03-24 | 2014-05-28 | 宜宾五粮液股份有限公司 | Analyzing and detecting method of flavor compound in white spirit |
| CN103969391A (en) * | 2014-05-23 | 2014-08-06 | 江南大学 | Method for determining volatile components in millet wine |
| CN104237435A (en) * | 2014-09-03 | 2014-12-24 | 上海应用技术学院 | Method for rapidly analyzing aroma components of distilled spirit |
| CN104849390A (en) * | 2015-05-29 | 2015-08-19 | 安徽古井贡酒股份有限公司 | Method for determining chemical composition in white spirit by adopting comprehensive two-dimensional gas chromatography-time of flight mass spectrometry |
| CN106018649A (en) * | 2016-07-14 | 2016-10-12 | 上海应用技术学院 | Identification method of nitrogen-containing compounds in Maotai |
| CN106018650A (en) * | 2016-07-14 | 2016-10-12 | 上海应用技术学院 | Method for identifying nitrogen-containing compound in kaoliang spirit |
| CN106124681A (en) * | 2016-07-14 | 2016-11-16 | 上海应用技术学院 | The authentication method of nitrogen-containing compound in a kind of Guo Jiao 1573 （The First Cellar in China） wine |
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| CN106198803A (en) * | 2016-07-14 | 2016-12-07 | 上海应用技术学院 | The authentication method of nitrogen-containing compound in a kind of blue rose whiskey cocktail |
| CN106226419A (en) * | 2016-07-14 | 2016-12-14 | 上海应用技术学院 | The authentication method of nitrogen-containing compound in a kind of Shuijingfang wine |
| CN106248818A (en) * | 2016-07-14 | 2016-12-21 | 上海应用技术学院 | The authentication method of nitrogen-containing compound in a kind of purple grape brandy cocktail |
| CN106770707A (en) * | 2016-11-15 | 2017-05-31 | 国家烟草质量监督检验中心 | The screening method of volatile organic matter in a kind of quick-fried pearl of cigarette filter |
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| CN107328876A (en) * | 2017-06-29 | 2017-11-07 | 安徽瑞思威尔科技有限公司 | A kind of method of volatile sulfur compounds in economic Quantitative detection white wine |
| CN107462624A (en) * | 2017-06-30 | 2017-12-12 | 江苏大学 | The rapid assay methods of main ester type compound content in a kind of white wine base liquor |
| CN107462624B (en) * | 2017-06-30 | 2020-08-28 | 江苏大学 | Method for rapidly determining content of main ester compounds in base liquor of white spirit |
| CN108181390A (en) * | 2017-12-21 | 2018-06-19 | 北京工商大学 | The quantitative detecting method of sulfur-containing compound in a kind of white wine |
| CN108181390B (en) * | 2017-12-21 | 2021-04-20 | 北京工商大学 | Quantitative detection method for sulfur-containing compounds in white spirit |
| CN109374759A (en) * | 2018-09-12 | 2019-02-22 | 北京工商大学 | A kind of method for concentration based on white wine liquid-liquid extraction |
| CN109959734A (en) * | 2019-03-21 | 2019-07-02 | 湖北工业大学 | The detection method of aroma compound in a kind of mixed-flavouring liquor |
| CN110927268A (en) * | 2019-11-25 | 2020-03-27 | 宜宾五粮液股份有限公司 | Method for acquiring and analyzing special aroma in white spirit |
| CN110927268B (en) * | 2019-11-25 | 2022-06-21 | 宜宾五粮液股份有限公司 | Method for obtaining and analyzing special aroma in white spirit |
| CN111024872A (en) * | 2019-12-25 | 2020-04-17 | 济南趵突泉酿酒有限责任公司 | Method for rapidly detecting 3-methylthio propanol in sesame-flavor liquor |
| CN111024872B (en) * | 2019-12-25 | 2022-06-03 | 济南趵突泉酿酒有限责任公司 | Method for rapidly detecting 3-methylthio propanol in sesame-flavor liquor |
| CN111398524A (en) * | 2020-04-01 | 2020-07-10 | 北京燕京啤酒股份有限公司 | Beer key flavor component identification threshold and evaluation method for harmony of beer key flavor component identification threshold and hop aroma |
| WO2022016683A1 (en) * | 2020-07-20 | 2022-01-27 | 中山大学 | Laser ionization system for combined use of solid-phase microextraction and time of flight mass spectrometry |
| CN113049631A (en) * | 2021-03-24 | 2021-06-29 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction method for quantitative analysis of thermogravimetric escaping substances |
| CN113049631B (en) * | 2021-03-24 | 2022-10-04 | 海南红塔卷烟有限责任公司 | Instillation micro-extraction method for quantitative analysis of thermogravimetric escaping substances |
| CN113933428A (en) * | 2021-07-29 | 2022-01-14 | 杨晓军 | Quantitative analysis method for flavor substances in soy sauce flavor type round base liquor |
| CN113917061A (en) * | 2021-10-22 | 2022-01-11 | 贵州大学 | Detection and identification method for volatile substances of Maotai-flavor base liquor |
| CN114062556A (en) * | 2021-11-19 | 2022-02-18 | 泸州老窖集团有限责任公司 | Carbon isotope composition detection method for white spirit flavor substances |
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| CN114384169A (en) * | 2021-12-14 | 2022-04-22 | 贵州茅台酒股份有限公司 | Method for rapidly analyzing volatile flavor substances in white spirit based on large-volume sample injection static headspace gas chromatograph-mass spectrometer |
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