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Quantification ethyl carbamate in wines using reaction-assisted-extraction with 9-xanthydrol and detection by heart-cutting multidimensional gas chromatography-mass spectrometry
Analytica Chimica Acta ( IF 6.2 ) Pub Date : 2018-02-01 , DOI: 10.1016/j.aca.2017.11.022
Qiqi Tu , Wanshu Qi , Junbo Zhao , Li Zhang , Yinlong Guo

9-Xanthydrol was introduced as an assisted-extraction-reagent to quantify ethyl carbamate (EC) in wines by heart-cutting multidimensional gas chromatography coupled with mass spectrometry (MDGC-MS). 9-Xanthydrol could help to increase the extraction efficiency, because it could react with ethyl carbamate to form the low-polar product, which facilitated the transfer of ethyl carbamate into organic phase. Then the reaction product was decomposed in high temperature, so ethyl carbamate could be obtained again in injector port. Heart-cutting multidimensional gas chromatography coupled with mass spectrometry was used not only for avoiding 9-xanthydrol interference but also for getting a larger volume injector, higher sensitivity and lower limit of detection. The method was optimized and validated in terms of sample volume, sodium chloride, the acid concentration, the 9-xanthydrol concentration and the reaction time. Good linear relationship (R2 = 0.9998) over the concentration range of 2.00 μg L-1 - 200.00 μg L-1 was obtained. The limit of detection (LOD, 0.02 μg L-1) and quantification (LOQ, 0.10 μg L-1) were lower than previously reported. The RSDs of precision (repeatability and reproducibility) were lower than 8.15%, and the recovery (96.17-99.25%) and accuracy (99.21-110.93%) were validated as well. This methodology was applied to the quantification of ethyl carbamate in several different fermented wines with values ranging from 13.05 to 155.20 μg L-1.

中文翻译:

9-黄水醇反应辅助萃取法和中心切割多维气相色谱-质谱法检测葡萄酒中氨基甲酸乙酯的定量

引入 9-Xanthydrol 作为辅助提取试剂,通过中心切割多维气相色谱结合质谱 (MDGC-MS) 对葡萄酒中的氨基甲酸乙酯 (EC) 进行定量。9-Xanthydrol 有助于提高萃取效率,因为它可以与氨基甲酸乙酯反应形成低极性产物,这有助于氨基甲酸乙酯转移到有机相中。然后反应产物在高温下分解,在进样口再次得到氨基甲酸乙酯。中心切割多维气相色谱与质谱联用不仅可以避免9-xanthydrol干扰,还可以获得更大体积的进样器、更高的灵敏度和更低的检测限。该方法在样品体积、氯化钠、酸浓度、9-xanthydrol 浓度和反应时间。在 2.00 μg L-1 - 200.00 μg L-1 的浓度范围内获得了良好的线性关系 (R2 = 0.9998)。检测限(LOD,0.02 μg L-1)和定量限(LOQ,0.10 μg L-1)低于之前报道的。精密度(重复性和再现性)的 RSD 低于 8.15%,回收率(96.17-99.25%)和准确度(99.21-110.93%)也得到验证。该方法应用于几种不同发酵葡萄酒中氨基甲酸乙酯的定量,其值范围为 13.05 至 155.20 μg L-1。02 μg L-1) 和定量 (LOQ, 0.10 μg L-1) 低于先前报告的值。精密度(重复性和再现性)的 RSD 低于 8.15%,回收率(96.17-99.25%)和准确度(99.21-110.93%)也得到验证。该方法应用于几种不同发酵葡萄酒中氨基甲酸乙酯的定量,其值范围为 13.05 至 155.20 μg L-1。02 μg L-1) 和定量 (LOQ, 0.10 μg L-1) 低于先前报告的值。精密度(重复性和再现性)的 RSD 低于 8.15%,回收率(96.17-99.25%)和准确度(99.21-110.93%)也得到验证。该方法应用于几种不同发酵葡萄酒中氨基甲酸乙酯的定量,其值范围为 13.05 至 155.20 μg L-1。
更新日期:2018-02-01
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