CN100549690C - The application of comprehensive two dimensional gas chromatography analytical technology in the local flavor beer development - Google Patents
The application of comprehensive two dimensional gas chromatography analytical technology in the local flavor beer development Download PDFInfo
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- CN100549690C CN100549690C CNB2007100518947A CN200710051894A CN100549690C CN 100549690 C CN100549690 C CN 100549690C CN B2007100518947 A CNB2007100518947 A CN B2007100518947A CN 200710051894 A CN200710051894 A CN 200710051894A CN 100549690 C CN100549690 C CN 100549690C
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Abstract
The application of comprehensive two dimensional gas chromatography analytical technology in the local flavor beer development, the gas componant in the local flavor beer that it is characterized in that the solid phase extraction enrichment is extracted detects the chemical composition of flavor substance in the local flavor beer by comprehensive two dimensional gas chromatography analysis and mass spectrophotometry coupling technique.Advantage of the present invention is: the present invention can obtain hundreds of beer flavor compositions, is used to make up the beer flavoring substances fingerprints database, finishes the evaluation to beer product perfect degree in auxiliary control of conventional production run quality and new product development process.Beer flavoring substances fingerprints database according to making up can be used for developing high-quality local flavor beer new product; Expanded the comprehensive two dimensional gas chromatography application.
Description
Technical field
The present invention relates to local flavor beer development field.
Background technology
The flavor substance of beer is of a great variety, and content is low, contains 2,000 multiple components such as multiple organism such as alcohols, aldehydes, ester class, ketone, acids, sulfide, aromatic substance and inorganic ions.Wherein moisture about 92%, alcohol is about 3 ~ 4%, and flavor ingredient contains 3% etc. approximately.The content of all kinds of flavor substances and level are to the odor type and the quality decisive role of beer.So must identify to the composition of beer product.Adopt suitable method to measure the beer flavor composition, making up the beer flavoring substances fingerprints database is the gordian technique means that each big beer brewery groups of the world carries out the quality control of high level.About beer flavor constituent analysis technology, retrieval is known according to current paper; Adopt static head space (SHS) the earliest, develop into solid-phase microextraction (SPME), one dimension gas chromatography (GC)/methods such as mass spectrum (MS) coupling then.Gas chromatography has obtained using widely in fields such as oil, chemical industry, geology, environmental protection as a kind of important analysis volatility and the instrument of half volatile organic compound.But, number of components is being reached several thousand even complex system up to ten thousand when analyzing, traditional one dimension chromatogram (1DGC) is not only time-consuming, and because peak capacity is not enough, overlap of peaks is very serious, the multidimensional piece-rate system is as: high performance liquid chromatography-gas chromatography coupling (HPLC-GC), supercritical fluid chromatography-gas chromatography coupling (SFC-GC) and common heartcut formula two dimension chromatogram (GC-GC) etc., also can only realize separation, can't carry out qualitative accurately and quantitative each component to the part components of interest.The beginning of the nineties, Liu and Phillips proposed the comprehensive two dimensional gas chromatography (method of GC * GC), a kind of real quadrature piece-rate system is provided, it is that different and mutual independently two chromatographic columns of separating mechanism are combined into two-dimensional gas chromatography in the mode of contacting, each cut after the 1st chromatographic column (non-polar column) separated, focus on the back through modulator and enter in the 2nd chromatographic column (polar column) with pulse mode and further separate, the orthogonalization of the change realization gas chromatography stalling characteristic by temperature and polarity.GC * GC has peak capacity big (being two posts products of peak capacity separately), characteristics such as analysis speed is fast, resolution is high, family's separation, thereby this method has the incomparable advantage of other method aspect the analysis of complex system, more and more be subjected to vast chromatogram worker's attention, studying expansion comprehensive two dimensional gas chromatography The Application of Technology field.The analyzing and testing that also the comprehensive two dimensional gas chromatography technology is not used for beer flavoring substances at present both at home and abroad.
Summary of the invention
Purpose of the present invention is exactly at the deficiency that also the comprehensive two dimensional gas chromatography technology is not used for the analyzing and testing of beer flavoring substances at present both at home and abroad, and the application of comprehensive two dimensional gas chromatography analytical technology in the local flavor beer development is provided, the gas componant in the local flavor beer that it is characterized in that the solid phase extraction enrichment is extracted detects the chemical composition of flavor substance in the local flavor beer by comprehensive two dimensional gas chromatography analysis and mass spectrophotometry coupling technique; Its operation steps is:
1), at first, adopts the method for solid-phase microextraction that beer sample is carried out pre-service, the gas componant enrichment in the local flavor beer is concentrated sampling by dimethyl silicone polymer/divinylbenzene extracting head; Adopt dimethyl silicone polymer/divinylbenzene (PDMS/DVB) extracting head, salt adding amount 4-4.5g, extraction temperature 40-60 ℃, equilibration time 20-30min, extraction time 20-40min;
2), the sample of extraction is separated by comprehensive two dimensional gas chromatography, detect by mass spectrophotometry, qualitative, quantitative makes some be difficult for detected but the big micro constitutent component of flavor quality influence is also come out by analysis again; GC * GC column system adopts DB-Petro (100%dimethylpolysiloxane) and DB-17ht (50%phenylmethylpolysiloxane) dual column system; Injector temperature: 250 ℃; Press before the post: 600kpa, constant voltage; Carrier gas: helium, purity 99.9995%; Split ratio: 1: 30; Sample size: 5 μ l; Modulation period: 5s; The Cheng Sheng condition: 40 ℃ (1min) is raised to 220 ℃ (30min) with 3 ℃/min; FID frequency acquisition: 100Hz; TOFMS frequency acquisition and acquisition range: 50Hz, 35-500u; Ion source temperature: 220 ℃; Transmission line temperature: 250 ℃;
3), data processing.Above-mentioned analysis result is generated and handled by Transform and Zoex software, adopt NIST/EPA/NIH version 2.0 spectrogram library searchings, all qualitative results generate the peak table automatically, further handle obtaining qualitative results, again by calculating the relative quantification result of each component concentration.
Advantage of the present invention is: the present invention can obtain hundreds of beer flavor compositions, is used to make up the beer flavoring substances fingerprints database, finishes the evaluation to beer product perfect degree in auxiliary control of conventional production run quality and new product development process.Beer flavoring substances fingerprints database according to making up can be used for developing high-quality local flavor beer new product; Expanded the comprehensive two dimensional gas chromatography application.
Embodiment
(1) experimental apparatus and experiment condition
1. instrument comprehensive two dimensional gas chromatography system is HP6890 gas chromatograph (the Agilent Technologies Wilmington by band hydrogen flame detector (FID), DE is USA) with KT-2001 type cold spray modulator (Zoex Corp., Lincoln, NE USA) forms.(MI USA) adopts 70eV electron impact ionization source to Pegasus III type mass spectrometer for Leco Corporation, St.Joseph.
2. experiment condition
GC * GC column system adopts DB-Petro (100%dimethylpolysiloxane) and DB-17ht (50%phenylmethylpolysiloxane) dual column system; Injector temperature: 250 ℃; Press before the post: 600kpa, constant voltage; Carrier gas: helium, purity 99.9995%; Split ratio: 1: 30; Sample size: 5 μ l; Modulation period: 5s; The Cheng Sheng condition: 40 ℃ (1min) is raised to 220 ℃ (30min) with 3 ℃/min; FID frequency acquisition: 100Hz; TOFMS frequency acquisition and acquisition range: 50Hz, 35-500u; Ion source temperature: 220 ℃; Transmission line temperature: 250 ℃.
Extraction conditions: adopt dimethyl silicone polymer/divinylbenzene (PDMS/DVB) extracting head, salt adding amount 4-4.5g, extraction temperature 40-60 ℃, equilibration time 20-30min, extraction time 20-40min.
(2) comprehensive two dimensional gas chromatography technical measurement beer flavor composition operation steps:
1, at first, adopt the method for solid-phase microextraction that beer sample is carried out pre-service.By dimethyl silicone polymer/divinylbenzene (PDMS/DVB, 85 μ m) extracting head the gas componant enrichment in the local flavor beer is concentrated sampling.
2, the sample with extraction separates by comprehensive two dimensional gas chromatography, detects qualitative, quantitative again by mass spectrophotometry.Make some be difficult for detected but flavor quality influenced big micro constitutent component also to be come out by analysis.
3, data processing.Above-mentioned analysis result is generated and handled by Transform and Zoex software, adopt NIST/EPA/NIH version 2.0 spectrogram library searchings, all qualitative results generate the peak table automatically, further handle obtaining qualitative results.Again by calculating the relative quantification result of each component concentration.
Adopt common solid-phase microextraction-gas chromatography/mass spectrometry (SPME-GC/MS) technology that the ordinary beer of the various brands of golden dragon's fountain is carried out the flavor components analysis, obtain tens kinds of beer flavor compositions and corresponding fingerprint spectrogram; (GC * GC) the beer flavor composition is carried out higher level separation detection obtains hundreds of flavor substances, for the foundation of golden dragon's fountain beer flavoring substances database is laid a good foundation to adopt comprehensive two dimensional gas chromatography/mass spectrometric hyphenated technique of the present invention; And it is used for the evaluation of local flavor beer new product development process product special flavour material, and the adjustment of further quality of assistance control, production technology.Owing to used this technology, promoted the quality of the local flavor beer product that " Yingbo Jinlongquan Beer (Hubei) Co., Ltd. " developed.
Novelty assessment report shows that the detection that is used for beer flavoring substances with the comprehensive two dimensional gas chromatography technology belongs to domestic initiation.
Claims (1)
1, the application of comprehensive two dimensional gas chromatography analytical technology in the local flavor beer development, gas componant in the local flavor beer that it is characterized in that the solid phase extraction enrichment is extracted detects the chemical composition of flavor substance in the local flavor beer by comprehensive two dimensional gas chromatography analysis and mass spectrophotometry coupling technique, and its operation steps is:
1), at first, adopts the method for solid-phase microextraction that beer sample is carried out pre-service, the gas componant enrichment in the local flavor beer is concentrated sampling by dimethyl silicone polymer/divinylbenzene extracting head; Adopt dimethyl silicone polymer/divinylbenzene (PDMS/DVB) extracting head, salt adding amount 4-4.5g, extraction temperature 40-60 ℃, equilibration time 20-30min, extraction time 20-40min;
2), the sample of extraction is separated by comprehensive two dimensional gas chromatography, detect by mass spectrophotometry, qualitative, quantitative makes some be difficult for detected but the big micro constitutent component of flavor quality influence is also come out by analysis again; GC * GC column system adopts DB-Petro (100%dimethylpolysiloxane) and DB-17ht (50%phenylmethylpolysiloxane) dual column system; Injector temperature: 250 ℃; Press before the post: 600kpa, constant voltage; Carrier gas: helium, purity 99.9995%; Split ratio: 1: 30; Sample size: 5 μ l; Modulation period: 5s; The Cheng Sheng condition: 40 ℃ (1min) is raised to 220 ℃ (30min) with 3 ℃/min; FID frequency acquisition: 100Hz; TOFMS frequency acquisition and acquisition range: 50Hz, 35-500u; Ion source temperature: 220 ℃; Transmission line temperature: 250 ℃;
3), data processing: above-mentioned analysis result is generated and handled by Transform and Zoex software, adopt NIST/EPA/NIH version 2.0 spectrogram library searchings, all qualitative results generate the peak table automatically, further handle and obtain qualitative results, again by calculating the relative quantification result of each component concentration.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102095826B (en) * | 2010-12-27 | 2014-06-04 | 广州珠江啤酒股份有限公司 | Method for detecting aging flavor substances in beer |
| CN102279230A (en) * | 2011-05-12 | 2011-12-14 | 西北农林科技大学 | Method for establishing volatile ingredient fingerprint map of agricultural product and processed product of agricultural product |
| CN102636609B (en) * | 2012-04-13 | 2014-04-02 | 中国石油天然气股份有限公司 | GC*GC (comprehensive two-dimensional gas chromatography) method for hydrocarbons in crude oil or sedimentary organic matters |
| CN102692363B (en) * | 2012-05-22 | 2014-07-02 | 中国石油天然气股份有限公司 | Method for forecasting crude oil viscosity before oil production test of exploratory well |
| CN102879496B (en) * | 2012-09-28 | 2014-04-02 | 四川剑南春（集团）有限责任公司 | Method for researching on bouquet of residue white spirit in wineglass |
| 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 |
| CN103995078B (en) * | 2014-05-28 | 2016-04-13 | 天津出入境检验检疫局动植物与食品检测中心 | 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 |
| CN104034836A (en) * | 2014-05-28 | 2014-09-10 | 天津出入境检验检疫局动植物与食品检测中心 | 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 |
| CN104849390B (en) * | 2015-05-29 | 2016-05-04 | 安徽瑞思威尔科技有限公司 | A kind of method of applying component in the qualitative white wine of comprehensive two dimensional gas chromatography-flight time mass spectrum coupling |
| CN110514757A (en) * | 2019-08-16 | 2019-11-29 | 江南大学 | A kind of method of Volatile flavor components in fast resolving white wine |
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