同位素内标-超高效液相色谱-高分辨质谱法测定酒醅中氨基甲酸乙酯

Determination of ethyl carbamate in fermented grains by isotope internal standard-ultra performance liquid chromatography-high resolution mass spectrometry

中文关键词:  氨基甲酸乙酯  酒醅  同位素内标法  超高效液相-高分辨质谱法  基质效应

英文关键词:ethyl carbamate  fermented grains  isotope internal standard method  ultra performance liquid chromatography-high resolution mass spectrometry  matrix effects

中文摘要:

      目的 建立同位素内标法结合超高效液相色谱-高分辨质谱法检测酒醅中氨基甲酸乙酯(ethyl carbamate, EC)含量的分析方法。方法 酒醅样品经超纯水超声提取离心过滤后, 以0.10%甲酸水溶液-甲醇溶液为流动相梯度洗脱, 通过Hypersil GOLD Amino色谱柱分离目标物, 在电喷雾正离子模式下采用一级全扫模式内标法定量分析。结果 同位素内标定量法能有效补偿样品中基质干扰, EC含量在4.00~300.00 μg/L质量浓度范围内线性关系良好(r2=0.9993), 定量限为6.25 μg/kg, 检出限为3.75 μg/kg。实际样品加标回收率为85.17%~97.40%, 相对标准偏差为1.12%~4.11%。结论 该方法线性、准确度和精密度均满足GB/T 27417—2017《化学分析方法确认和验证指南》的要求, 适用于酒醅中EC的分析检测。

英文摘要:

      Objective To establish an analytical method for ethyl carbamate (EC) in fermented grains by isotope internal standard method combined with ultra performance liquid chromatography-high resolution mass spectrometry. Methods Fermented grains were extracted by ultrapure water, filtered after centrifugation. The 0.10% formic acid aqueous solution and methanol solution were used as mobile phase for gradient elution. The samples were separated by Hypersil GOLD Amino chromatographic column; the internal standard method with full mass scan mode was used for quantitative analysis in electrospray positive ion mode. Results The matrix interference was effectively compensated by internal standard quantitative method. The calibration curve of EC showed good linearity in the range of 4.00?300.00 μg/L (r2=0.9993), the limit of quantification was 6.25 μg/kg, and the limit of detection was 3.75 μg/kg. The recoveries of the actual samples ranged from 85.17%?97.40%, and range of relative standard deviations were 1.12%?4.11%. Conclusion The linearity, accuracy and precision of this method meet the requirements of GB/T 27417—2017 Guidelines for the confirmation and verification of chemical analysis methods, and it is suitable for the detection of EC in fermented grains.