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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0.45μm.有机相滤膜,气相色谱-质谱测定。选择VOCOL石英毛细管柱(60m×0.32 mm,1.8μm)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/m L浓度范围内呈良好的线性关系,相关系数r~2=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。
Objective To establish a gas chromatography-mass spectrometry method for the determination of acrylonitrile in fresh shellfish. Methods The samples were extracted by N, N - dimethylformamide (DMF) and centrifuged at 0.45μm after high speed centrifugation. The organic phase was separated by gas chromatography - mass spectrometry. The VOCOL quartz capillary column (60m × 0.32mm, 1.8μm) was used to separate ion bombardment ion source (EI). The selected ions were m / z 53, m / z 52 and m / z 51 / z 53), external standard method. Results The linear range of acrylonitrile was 10 ~ 200 ng / m L, the correlation coefficient r ~ 2 = 0.9999, the recovery was 87.2% ~ 96.1%, and the relative deviation RSD was 4.4% -7.3% (n = 6 ); The detection limit was 0.02 mg / kg and the limit of quantification was 0.05 mg / kg. Conclusion The method has the advantages of simple pretreatment, high accuracy and precision, greatly saving the testing time and cost on the basis of ensuring the reliable analysis results, and rapidly and accurately analyzing the residual amount of acrylonitrile in fresh shellfish.