Detection And Analysis Of Ethyl Carbamate And Biogenic Amine In Wines From Hexi Corridor

Ethyl carbamate?EC?and biogenic amines?BA?are metabolic by-products produced by microorganisms during wine brewing.Both substances have potential toxic effects on human health.In this paper,Based on liquid-liquid extraction pretreatment,sodium chloride salting-out assisted dichloromethane extraction and concentration of EC in wine matrix,combined with gas chromatography-mass spectrometry?GC-MS?detection,and EC was accurately quantified by deuterium isotope?EC-D5?internal standard method.At the same time,BA in wine was extracted by QuEChERS pretreatment and detected by UPLC-MS/MS.The seven biogenic amines were quantified accurately with 1,7-diaminoheptane as internal standard.On the basis of establishing two detection methods,the quantitative and analysis of EC and BA in the wines of Hexi Corridor production area were carried out for the first time.The correlation between the known characteristic parameters of wine and the concentration levels of EC and BA was analyzed,and the safety of wine in this wine region was evaluated.The conclusion was drawn as follows:1.When 5 mL of the test sample was treated with 15 mL of dichloromethane and 1.2 g of NaCl,the best extraction effect was obtained and the solvent consumption was less.At the same time,the test method obtained in the test has a good correlation in the range of 5²00?g/L?R²?0.9985?,the recovery rate?84.18%¹11.24%?,sensitivity?LOD 0.8?g/L,LOQ2.64?g/L?and precision?RSD?3.78%?all meet the method validation criteria.2..Mainly based on QuEChERS pretreatment,without derivatization,adjust the pH of wine to 12 by NaOH,add 1 g of NaCl and 2 g of anhydrous Na₂CO₃,and extract with 10 mL of n-butanol:chloroform?v/v:1/1?.No purification step.Detection was carried out by UHPLC-MS/MS?ESI+?.The method has a good linear relationship?R²?0.9903?,recovery?81.89%⁹9.61%?,sensitivity?LOD,0.50¹.00?g/L;LOQ,1.65³.30?g/L?in the range of0.5⁸00?g/L.The precision?RSD?9.74%?all the verification indicators are in line with the methodological verification standards.3.Quantitative detection and analysis of EC in 81 wines of the Hexi Corridor.The results showed that EC was 100%detected as an endogenous compound.China has not yet set a limit standard for EC in wine.Compared with the International Food and Agriculture Organization?FAO?limit standard of 20?g/L,18 wines exceed this value.Most of the 18wines have a shelf life of more than 10 years.4.Quantitative analysis of 7 biogenic amines in 81 wines showed that tryptamine was not detected,while the other six biogenic amines existed in varying degrees,putrescine>histamine>tyramine>2-pHenylethylamine>cadaverine>hexamine.Putrescine,tyramine and 2-pHenylethylamine were detected in all samples,but histamine,cadaverine and hexamine were not detected in a few samples.none of the 81 wines exceeded the limits or toxic doses.5.A correlation analysis was performed between the measured BA and EC concentration values and the characteristic parameters of the wine.The results showed that the concentration of EC increased with the increase of wine age;there was a significant positive correlation between the concentration of phenethylamine in wine and EC concentration,the concentration of hexylamine and cadaverine?P<0.01?,that is,a wine When the concentration of phenethylamine was higher,the EC,cadaverine and hexylamine contained in the concentration also showed a certain concentration;there was a significant positive correlation between the concentration of tyramine in wine and the concentration of histamine?P<0.01?,there was also a significant correlation with cadaverine?P<0.05?.At the same time,the total biogenic amine concentration level in wine is mainly determined by the concentration of putrescine,histamine and tyramine.