气相色谱-质谱法测定新鲜贝类中丙烯腈的残留量

Determination of acrylonitrile residue in fresh shellfish by gas chromatography-mass spectrometry

中文关键词:  丙烯腈  气相色谱-质谱法  贝类

英文关键词:acrylonitrile  gas chromatography-mass spectrometry  shellfish

中文摘要:

      目的 建立新鲜贝类中丙烯腈残留量检测的气相色谱-质谱分析方法。方法 样品经N,N-二甲基甲酰胺(DMF)超声提取, 高速离心后, 过0.45 μm.有机相滤膜, 气相色谱-质谱测定。选择VOCOL石英毛细管柱(60 m×0.32 mm, 1.8 μm)分离, 电子轰击离子源(EI)离子化, 选择监测离子为m/z 53, m/z 52, m/z 51(其中定量离子为m/z 53), 外标法定量。结果 丙烯腈在10~200 ng/mL浓度范围内呈良好的线性关系, 相关系数r2=0.9999; 回收率为87.2%~96.1%, 相对偏差RSD为4.4%~7.3%(n=6); 方法检出限为0.02 mg/kg, 定量限为0.05 mg/kg。结论 本方法前处理简单, 准确度及精密度高, 在保证分析结果可靠的基础上大大的节省了检测时间及成本, 可快速, 准确地对新鲜贝类中丙烯腈的残留量进行分析。

英文摘要:

      Objective To establish a method for determination of acrylonitrile residue in fresh shellfish by gas chromatography–mass spectrometry (GC-MS). Methods Samples were determined by GC-MS after extraction by N,N - dimethyl formamide (DMF) combined with ultrasonic, high speed centrifugation and filtration by 0.45 μm organic phase membrane. Compounds were separated by VOCOL quartz capillary column (60 m×0.32 mm, 1.8 μm) and ionized by electron impact ionization source (EI), selected ion monitoring (SIM) was used and the selected ions were m/z 53, m/z 52, m/z 51 (m/z 53 was the quantitative ion), with external standard method for quantitation. Results The acrylonitrile had a good linear relationship in the range of 10 ~200 ng/mL, with the correlation coefficient r2=0.9999. The recoveries were 87.2%~96.1%, relative standard deviations (RSDs) were 4.4%~7.3% (n=6), the limit of detection of the method was 0.02 mg/kg and the limit of quantitation of the method was 0.05 mg/kg. Conclusion This method can analyze the acrylonitrile residue in fresh shellfish quickly and accurately, for its simple preparation, high accuracy and high precision. It can greatly save testing time and cost on the basis of the reliable results.