Determination Of Ethyl Carbamate In Liquor By Gas Chromatography-mass Spectrometry(GC-MS)

Objective: Establishing an accurate and efficient method whichcan apply to a large number of samples for determining ethyl carbamate inliquor. Methods:(1) Chromatography and mass spectrometry conditions: UseGas chromatography-Mass spectrometry, which the instrument comes fromShimadzu GC2010-QB2010. The chromatographic column is AgilentDB-WAX30m, diameter is0.32um, film thickness is0.25um.(2)Samplepurification methods: use solid-phase extraction with SUPELCO and withfilling of alkaline diatomite and PSA. Study the purification results in alkalinediatomite and PSA respectively or both of them. Elution: study the elutingeffects of dichloromethane、diethyl ether、ethyl acetate-diethyl ether（5%）,respectively, with recovery rate as evaluation index.(3) Method verification: thestudy of linearity range、linear correlation coefficient、limit of detection、limitof quantitation、recovery rate、stability can be used to verify whether thismethod could apply to the detection of EC in wine.（4）Sample determination:take the method which is decided above to determine the content of EC in winein different regions of Luzhou city. Result：(1) Chromatography and massspectrometry conditions: external standard method: inlet temperature220℃,column temperature60℃keeping1min, raising the temperature to150℃withthe speed of5℃/min, keeping1min, then rising to240℃with the speed of10℃/min, keeping5min. EI ion source: ion source temperature230℃, detectorvoltage0.2kv, using SIM mode, quantitative ion62, qualitative ion74、89.(2) Sample purification methods is best with using solid-phase extractiontechnology with combination of alkaline diatomite and PSA: Getting2ml liquorsamples to Solid-phase extraction column with filling5ml alkaline diatomite,keeping adsorption still for10min, then15ml n-Hexane–eluting, discardingeluent. Vacuum pumps the column to dry, use25ml ethyl acetate-diethyl ether（5%）to elute, washing liquid could get purification after go through the smallcolumn with filling2ml PSA, and then use nitrogen(about0.5ml) to dry it withacetonitrile diluting to1ml(3)Method verification result: when concentration ofthis method locates0.085mg/L-1.694mg/L,r2=0.9973, repetitive testing RSDis3.9%,the limit of detection is2ug/L, limit of quantitation is7ug/L, therecovery is between80%and90%. The sample solution had a good stabilitywithin24hours.(4) Sample determination: The EC content in finished andsemi-finished wine is0-0.22mg/kg, in base liquor is0.05-0.37mg/kg, inmaotai-flavor liquor is0.05-0.11mg/kg. Conclusions：The merits of thismethod is convenient and quick with purification,it can handle more sampleswith just one time. What’s more, it is reliable to detect the content of EC inliquor,and the results are highly deserving popularization. Through thesample analysis, white wine with different processing existed differences incontent of EC. The EC content of the Jiang-flavor spirits is lower than that ofstrong-flavor spirits. The EC content in liquor with the same processingincreases with the pits of age.