Study On Characteristic Components In A Certain Brand Of Strong Aromatic Chinese Spirits

As one of three categories classified according to aroma characteristics of Chinese liquor,strong aromatic Chinese spirits is one of the largest output wines in China.Its mud-pit fermentation process is unique in winemaking in our country,and its flavour characteristic is the leader in the liquor industry.Taking a certain brand of strong aromatic Chinese spirit as the research subject,this thesis attempted to inquire the kinds and contents of micro constituents in different series of the liquor and summarize laws of characteristic components between different series of the liquor by applying different sample pretreatment methods combining with advanced detection methods.The research provides a foundation of controlling the quality of wines during the blending process.The author conducted the research from the following three aspects:1.Headspace technology(HS)and Headspace solid phase micro-extraction technique(HS-SPME)were applied to separate trace components in 3 series of the liquor respectively.GC-MS technique was used for conducting qualitative and semi-quantitative analysis of volatile components in the liquors.During the HS-SPME process,the effects of fiber membrane,equilibrium temperature,equilibrium time,extraction time and ammount of salt addition on extraction efficiency were observed and optimized.The optimized conditions were as follows:50/30 ?m DVB/CAR/PDMS fiber was selected,and the equilibrium temperature was held at 60?,the equilibrium time was maintained at 30 min,and extraction time was controlled at 40 min,finally 2 g NaCl was added in the sample.12 kinds of volatile components are detected in 3 series of liquors by HS-GC-MS.The dominant compounds are ethyl acetate,ethyl butyrate and lactate,and the content of them in 3 series of liquors base the following laws:1#<3#<2#(including lactate,ethyl acetate)?3#<2#<1#(ethyl butyrate).36 kinds of compounds were detected from wines by optimised HS-SPME-GC-MS.The major components are esters,alcohols and acetals;Ethyl caproate,ethyl valerate,ethyl octanoate and ethyl lactate occupy the main content of esters;the high content of furfural means sauce favor existed in Jiugui Liquor.The laws they presented in 3 series of liquors are as follows:1#<2#<3#(including est-A,ethyl caproate,ethyl oenanthate,and alcohols),1#<3#<2#(including est-B,est-C,furfural,acetals).The different content of est-A,est-B and est-C in 3 series of liquors can be the basis of distinguishing wines.2.vortex-assisted liquid-liquid micro-extraction method was established to separate and enrich the micro compounds in wine.Response surface methodology was applied to optimize the condition of extraction,including extraction time,volume of extractant and concentration of wine.The optimized conditions were as follows:wine at a concentration of 52.5%was added dichloromethane with a volume of 550 ?L,and extracted for 20 min with the amount of NaCl at 2 g.The linear correlation coefficient of quantitative materials were greater than 0.99,and the relative standard deviations were quantified within 12%,the recovery of all quantitative compounds were range from 70%to 113%,meeting the requirement of precisely quantifying those compounds.60 kinds of compounds are detected from wines,including 27 species of esters,11 kinds of acids,6 species of alcohols,4 kinds of acetals,4 kinds of aldehyde compounds and others.The laws they presented in 3 series of liquors are as follows:1#<2#<3#(inciuding ethyl caproate,est-A,ethyl heptanoate,est-B,butyric acid,pentanoic acid,hexanoic acid,aid-D),1#<3#<2#(including est-C,est-E),2#<3#<1#(aci-F).The different content of ald-D,est-E and aci-F in 3 series of liquors can be the basis of distinguishing wines.3.High performance liquid chromatography-triple quadruple mass spectrometer technique was applied to detected sodium cyclamate in wine.The retention time of sodium cyclamate was optimized by selecting different types and proportion of mobile phase.The Fragmentor Voltage and Collision Energy were optimized for obtaining higher abundance of product ion.The conditions of instrument determined as follows:isocratic elution with 85 percentage of mobile phase A(0.1%formic acid aqueous solution with ammonium formate at a concentration of 5 millimoles)and 15 percentage of mobile phase B(acetonitrile),fragmentor voltage and collision energy were at 110 V and 25 eV respectively.The linear correlation coefficient of sodium cyclamate was 0.9981,and the concentration range was 10?1500?g/L.The limit of detection was 8.26 ?g/L,and the recovery was between 85%and 104%(RSD<5%).The concentrations of sodium cyclamate in 3 series of liquors are 116.40,110.97 and 171.13?g/L,respectively.