CN100432668C - Method for determining volatile element in shaoxing wine - Google Patents
Method for determining volatile element in shaoxing wine Download PDFInfo
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- CN100432668C CN100432668C CNB2007100202516A CN200710020251A CN100432668C CN 100432668 C CN100432668 C CN 100432668C CN B2007100202516 A CNB2007100202516 A CN B2007100202516A CN 200710020251 A CN200710020251 A CN 200710020251A CN 100432668 C CN100432668 C CN 100432668C
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Abstract
A method to detect volatile component in yellow wine belongs to technical field of yellow wine specialty analysis. The invention adopts coupled technique of roof solid phase extraction and gas phase chromatography-mass spectrum to make qualitative and semi-quantitative analysis of volatile component in yellow wine. The method can detect volatile compound in yellow wine quickly and estimate its proportion in all volatile compound initiatively. Roof solid phase extraction can complete under normal temperature without organic solvent, which avoid producing new compound during analyzing and enrich volatile component effectively. Mass spectrum detection can identify volatile component accurately to improve accuracy of the method. The invention has significance in researching micro constituent in yellow wine and improving its quality.
Description
Technical field
A kind of method of measuring volatile ingredient in the yellow rice wine belongs to the rice wine flavor analysis technical field, is specifically related to headspace solid-phase microextraction and gas chromatography-mass spectrography technology.
Background technology
Yellow rice wine is one of the most ancient in the world drinks, comes from China, and only state-owned it, with beer, grape wine and claim the world three Da Gu wine.The micro constitutent of yellow rice wine is very abundant, comprises alcohols, aldehydes, acids, ester type compound, sulfide, aromatics etc.The abstraction technique of yellow rice wine micro constitutent mainly contains at present: static head space method (Static headspace), liquid-liquid extraction method (Liquid-liquid extraction, LLE), the way of distillation (Distillation) etc., but these methods cut both ways, all there are some defectives, organic solvent as liquid-liquid extraction may have toxicity, contaminated environment, need sample size big, complex steps, consuming time, and can cause the variation of some chemical composition, particularly when carrying out the quantitative measurement of effumability material, be easy to generate, even lose some low-boiling point material than mistake.The vapour volume that static head space method major defect is a sample is excessive, influence the separation efficiency of chromatographic column, and some partly volatilize and difficult volatile aroma compound can't detect.Contain ethanol in the yellow rice wine, limited the application of the way of distillation; In addition, when distillation, easily produce some new compounds etc.
Solid-phase microextraction (Solid phase microextraction, SPME) be a kind of sample pretreatment concentration technique of novel concept, it has overcome the shortcoming of traditional extraction method, compare with other technologies, it is short to have easy, highly sensitive, reappearance and good linearity, sample preparation time, the analytic sample consumption is few, need not advantages such as organic solvent and environmental protection.Although domestic micro constitutent for yellow rice wine has been carried out some researchs, also do not utilize solid-phase microextraction and makings coupling technique that yellow rice wine micro constitutent is studied both at home and abroad.
Summary of the invention
(1) goal of the invention
The purpose of this invention is to provide a kind of method of measuring volatile ingredient in the yellow rice wine, method has adopted headspace solid-phase microextraction and gas chromatography-mass spectrography technology to measure volatile ingredient in the yellow rice wine.The headspace solid-phase microextraction technology need not the just effective volatile matter in the enriched sample of organic solvent, and highly sensitive, easy and simple to handle.
(2) technical scheme
The method of volatile ingredient in the mensuration yellow rice wine of the present invention, earlier with deionized water wine sample to be measured being diluted to final alcohol content is 6% (v/v), use headspace solid-phase microextraction technology enrichment volatile ingredient then, enter the gas chromatography-mass spectrum detecting device again the volatile ingredient in the yellow rice wine is carried out qualitative and semi-quantitative analysis.
The preparation of inner mark solution: sec-n-octyl alcohol (chromatographically pure) is purchased in Fluka.Sec-n-octyl alcohol inner mark solution concentration is 0.108mg/mL, is formulated in the absolute ethyl alcohol.
Volatile ingredient extracts: (Bellefonte PA) extracts volatility and semi-volatility component for Supelco, Inc. with 50/30 μ m DVB/CAR/PDMS extracting head.Be equipped with at 15ml that to add 6ml dilution back alcohol content in the head space bottle of miniature magnetic stirrer be the wine sample of 6% (v/v), 5 μ l inner mark solutions, 2.5g sodium chloride, screw the lid that is lined with the teflon silicagel pad, rotating speed with 500rpm in 50 ℃ of water-baths stirs balance 15min, insert 50/30 μ m DVB/CAR/PDMS extracting head, extraction absorption 30min under the condition of 50 ℃ and 500rpm.
Gas chromatography-mass spectrometry analysis process: after extraction finishes extracting head is inserted into the injection port of gas chromatography (AgilentGC 6890), at 250 ℃ of desorb 5min under the shunt mode not.With Agilent GC 6890-5975mass selective detector (MSD) sample is identified.Sample is by DB-Wax capillary column (long 30m, diameter 0.25mm, thickness 0.25 μ m, J﹠amp; W Scientific) separates.Temperature programme condition: 50 ℃ of column temperatures (keeping 0min); Speed with 20 ℃/min is warming up to 80 ℃ (keeping 0min); Speed with 3 ℃/min is warming up to 230 ℃ (keeping 0min) again.With the helium is carrier gas, and flow velocity is 2ml/min.Sample after the separation is identified with mass spectrum (Agilent 5975MSD).Mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 30amu-550amu.
The qualitative analysis of material: the mass spectrum of standard model and the retention index of standard model among mass spectrum by comparing unknown volatile compound and the NIST05a.L Database of retention index and AgilentTechnologies Inc., with the detected volatile compound of this qualitative affirmation.
The semi-quantitative analysis of material: the relative content that calculates volatile ingredient by semiquantitative method.
Semi-quantitative method: to confirmed volatile ingredient: by the ratio of the chromatographic peak area of testing compound and interior target chromatographic peak area with in the ultimate density that is marked in the wine multiply each other, obtain the relative concentration (this result do not consider the influence of other factors, suppose improvement factor be 1) of testing compound in yellow rice wine.
All experiments repeat 3 times, average as net result.
(3) beneficial effect
The volatile compound of the method that the present invention sets up in can the fast detecting yellow rice wine, and can tentatively judge its proportion size in all volatile compounds of yellow rice wine.The headspace solid-phase microextraction technology need not organic solvent, just can finish in the normal temperature scope, has avoided producing in the analytic process new compound, effectively enrichment volatile ingredient; Mass spectrum detection can identify volatile compound rapidly and accurately, has improved the accuracy of this method.The present invention is a micro constitutent in the further systematic study yellow rice wine, and is significant to improving the yellow rice wine quality.
Description of drawings
Beautiful 12 years old yellow rice wine gas chromatograms of Fig. 1 gold maple.
Fig. 2 Jin Fengte is with 5 years old yellow rice wine gas chromatograms of meal.
The excellent chrysanthemum of Fig. 3 shoal opens rich and honour 8 years old yellow rice wine gas chromatograms.
Embodiment
It is 6% (v/v) that beautiful 12 years old yellow rice wine of the golden maple of 12% (v/v) are diluted to final alcohol content with deionized water, draws 6ml wine sample and places 15mL head space bottle, adds 5 μ L inner mark solutions and 2.5g sodium chloride, screws lid.In 50 ℃ of water-baths, stir balance 15min, insert 50/30 μ m DVB/CAR/PDMS extracting head, under the condition of 50 ℃ and 500rpm, extract 30min with the rotating speed of 500rpm.Then extracting head is inserted the gas chromatography injection port, in 250 ℃ of desorb 5min under the shunt mode not.Adopt the DB-Wax capillary column to separate, set 50 ℃ of initial column temperatures (keeping 0min); Speed with 20 ℃/min is warming up to 80 ℃ (keeping 0min); Speed with 3 ℃/min is warming up to 230 ℃ (keeping 0min) again.With the helium is carrier gas, and flow velocity is 2ml/min.Sample after the separation is identified with mass spectrum (Agilent 5975MSD).Mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 30amu-550amu.Table 1 is the testing result of beautiful 12 years old yellow rice wine of golden maple.
The testing result of beautiful 12 years old yellow rice wine of table 1 gold maple
Embodiment 2
It is 6% (v/v) that the Jin Fengte of 14% (v/v) is diluted to final alcohol content with 5 years old yellow rice wine of meal with deionized water, draws 6ml wine sample and places 15mL head space bottle, adds 5 μ L inner mark solutions and 2.5g sodium chloride, screws lid.In 50 ℃ of water-baths, stir balance 15min, insert 50/30 μ m DVB/CAR/PDMS extracting head, under the condition of 50 ℃ and 500rpm, extract 30min with the rotating speed of 500rpm.Then extracting head is inserted the gas chromatography injection port, in 250 ℃ of desorb 5min under the shunt mode not.Adopt the DB-Wax capillary column to separate, set 50 ℃ of initial column temperatures (keeping 0min); With 20 ℃/min speed be warming up to 80 ℃ (keep 0min); Speed with 3 ℃/min is warming up to 230 ℃ (keeping 0min) again.With the helium is carrier gas, and flow velocity is 2ml/min.Sample after the separation is identified with mass spectrum (Agilent 5975 MSD).Mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 30amu-550amu.Table 2 is the testing result of Jin Fengte with 5 years old yellow rice wine of meal.
Table 2 Jin Fengte is with the testing result of 5 years old yellow rice wine of meal
Embodiment 3
The excellent chrysanthemum of the shoal of 10% (v/v) is opened rich and honour 8 years old yellow rice wine, and to be diluted to final alcohol content with deionized water be 6% (v/v), draws 6ml wine sample and place 15mL head space bottle, adds 5 μ L inner mark solutions and 2.5g sodium chloride, screws lid.In 50 ℃ of water-baths, stir balance 15min, insert 50/30 μ m DVB/CAR/PDMS extracting head, under the condition of 50 ℃ and 500rpm, extract 30min with the rotating speed of 500rpm.Then extracting head is inserted the gas chromatography injection port, in 250 ℃ of desorb 5min under the shunt mode not.Adopt the DB-Wax capillary column to separate, set 50 ℃ of initial column temperatures (keeping 0min); With 20 ℃/min speed be warming up to 80 ℃ (keep 0min); Speed with 3 ℃/min is warming up to 230 ℃ (keeping 0min) again.With the helium is carrier gas, and flow velocity is 2ml/min.Sample after the separation is identified with mass spectrum (Agilent 5975MSD).Mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 30amu-550amu.Table 3 is opened the testing result of rich and honour 8 years old yellow rice wine for the excellent chrysanthemum of shoal.
The excellent chrysanthemum of table 3 shoal opens rich and honour 8 years old yellow rice wine testing results
Claims (3)
1. method of measuring volatile ingredient in the yellow rice wine, it is characterized in that with deionized water wine sample to be measured being diluted to final alcohol content earlier is 6%v/v, use headspace solid-phase microextraction technology enrichment volatile ingredient then, enter the gas chromatography-mass spectrum detecting device again the volatile ingredient in the yellow rice wine is carried out qualitative and semi-quantitative analysis;
Headspace solid-phase microextraction: drawing the 6mL alcohol content is the wine sample of 6%v/v, add 5 μ L inner mark solutions, place 15mL head space bottle, add 2.5g sodium chloride again, screw lid, in 50 ℃ of water-baths, stir balance 15min, insert 50/30 μ m DVB/CAR/PDMS extracting head, under the condition of 50 ℃ and 500rpm, extract 30min with the rotating speed of 500rpm;
Used inner mark solution is the sec-n-octyl alcohol inner mark solution, and concentration is 0.108mg/mL, is formulated in the absolute ethyl alcohol;
The coupling of gas chromatography-mass spectrum detecting device is measured: after extraction finishes extracting head is inserted into the injection port of Agilent GC6890 gas chromatography, at 250 ℃ of desorb 5min under the shunt mode not; Sample is by long 30m, diameter 0.25mm, thickness 0.25 μ m, J﹠amp; The DB-Wax capillary column of W Scientific separates, the temperature programme condition: column temperature keeps 0min for 50 ℃; Speed with 20 ℃/min is warming up to 80 ℃ of maintenance 0min; Speed with 3 ℃/min is warming up to 230 ℃ of maintenance 0min again; With the helium is carrier gas, and flow velocity is 2ml/min; Sample after the separation is identified with Agilent 5975 MSD mass spectrums, mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 30amu-550amu.
2. method according to claim 1, it is characterized in that the qualitative analysis of volatile ingredient: the mass spectrum of standard model and the retention index of standard model among mass spectrum by comparing unknown volatile compound and the NIST05a.LDatabase of retention index and Agilent Technologies Inc., with the detected volatile compound of this qualitative affirmation.
3. method according to claim 1, it is characterized in that confirmed volatile ingredient is carried out semi-quantitative analysis: by the ratio of the chromatographic peak area of testing compound and interior target chromatographic peak area with in the ultimate density that is marked in the wine multiply each other, obtain the relative concentration of testing compound in yellow rice wine.
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101620206B (en) * | 2009-06-18 | 2011-09-21 | 浙江大学 | Method for detecting ethyl carbamate in yellow wine |
| CN102095809A (en) * | 2009-12-15 | 2011-06-15 | 青岛啤酒股份有限公司 | Analysis method for detecting pyrazine compounds in beer |
| CN101762658B (en) * | 2010-01-13 | 2012-05-23 | 江南大学 | Method for measuring volatility constituent in white wine |
| CN102331466B (en) * | 2011-07-25 | 2013-05-15 | 四川省宜宾五粮液集团有限公司 | Method for comprehensively testing fragrant components of crops |
| CN103969391A (en) * | 2014-05-23 | 2014-08-06 | 江南大学 | Method for determining volatile components in millet wine |
| CN106950299A (en) * | 2017-03-08 | 2017-07-14 | 浙江奇彩环境科技股份有限公司 | Method for n-octyl alcohol content in determination sample |
| CN108362760A (en) * | 2017-05-10 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of qualitative and semi-quantitative detection method of oxygen-containing acid group, a kind of monitoring method and application thereof of oxygen-containing acid group |
| CN107568221A (en) * | 2017-09-05 | 2018-01-12 | 浙江省农业科学院 | A kind of active compound based on aldehyde C-9 and n-octyl alcohol, striped rice borer attractant and application |
| CN108469486A (en) * | 2018-05-03 | 2018-08-31 | 江南大学 | Main higher alcohol in dispersive liquid-liquid microextraction gas-chromatography combination detection fermented wine |
| CN109781918B (en) * | 2019-01-11 | 2020-05-22 | 浙江大学 | Gas phase ion mobility spectrometry identification method for yellow rice wine produced by different enterprises |
| CN109725090B (en) * | 2019-03-16 | 2021-05-18 | 丁立平 | Gas chromatography-mass spectrometry combined method for measuring four trace phenylpropionic acids in water source water |
| CN109884213A (en) * | 2019-04-02 | 2019-06-14 | 上海应用技术大学 | A kind of method of quick analysis yellow rice wine key volatile compound |
| CN112834639B (en) * | 2020-12-31 | 2022-06-21 | 宜宾五粮液股份有限公司 | Series connection method of solid phase extraction columns for separating volatile ester flavor substances in white spirit |
| CN113917013B (en) * | 2021-09-30 | 2024-02-02 | 山东省葡萄研究院 | Method for measuring methanol and 5 higher alcohols in fruit distilled liquor by internal standard method |
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| US4656140A (en) * | 1983-11-18 | 1987-04-07 | Nakano Vinegar Co., Ltd. | Method for a measurement of alcohol concentration in acetic acid fermenting broth |
| CN1408840A (en) * | 2001-09-18 | 2003-04-09 | 上海神仙酒业有限公司 | Process and recipe of nutritive yellow rice wine |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4656140A (en) * | 1983-11-18 | 1987-04-07 | Nakano Vinegar Co., Ltd. | Method for a measurement of alcohol concentration in acetic acid fermenting broth |
| CN1408840A (en) * | 2001-09-18 | 2003-04-09 | 上海神仙酒业有限公司 | Process and recipe of nutritive yellow rice wine |
Non-Patent Citations (2)
| Title |
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