基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对 HS-SPME方法进行了优化,在酒精度12% vol、加NaCl 3 g、萃取温度70 ℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D5-氨基甲酸乙酯(D5-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500 μg/L范围内线性关系良好,回归系数(R2)>0.998,检出限为0.19 μg/L,定量限为0.64 μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。
李欣
,
杜娟
,
刘阳晴雪
,
吴刚
,
杨丽华
,
仇凯
,
常迪
,
屠振华
,
宋妍妍
,
周靖
,
刘冰
,
高红波
. SPME结合GC×GC-TOFMS测定白酒中的氨基甲酸乙酯[J]. 食品与发酵工业, 2023
, 49(7)
: 270
-274
.
DOI: 10.13995/j.cnki.11-1802/ts.032255
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.
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