Based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS), an accurate method was established for the determination of ethyl carbamate (EC) in Baijiu. In the experiment of optimizing HS-SPME, the response signal of the target substance was significantly improved under 12% vol, 3 g NaCl, 70 ℃ of extraction temperature and 40 min of extraction time. In this experiment, D5-ethyl carbamate (D5-EC) was used as the internal standard, and the sample solutions with different concentrations were quantitatively analyzed by GC×GC-TOFMS. The results showed that EC had a good linear relationship in the range of 10-500 μg/L, with the regression coefficient (R2) greater than 0.998, detection limit of 0.19 μg/L, quantitative limit of 0.64 μg/L, average recovery of 97.57%, and the precision of 8.66%. More importantly, there was no significant difference between the new method and the national standard method (P >0.05). As a result, this method has simple pretreatment and higher detection sensitivity, which provides a new method for automatic quantitative determination of EC in Baijiu.
LI Xin
,
DU Juan
,
LIU Yangqingxue
,
WU Gang
,
YANG Lihua
,
QIU Kai
,
CHANG Di
,
TU Zhenhua
,
SONG Yanyan
,
ZHOU Jing
,
LIU Bing
,
GAO Hongbo
. Determination of ethyl carbamate in Baijiu by SPME combined with GC×GC-TOFMS[J]. Food and Fermentation Industries, 2023
, 49(7)
: 270
-274
.
DOI: 10.13995/j.cnki.11-1802/ts.032255
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