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建立了亚临界水萃取(SCWE)及气相色谱-质谱(GC-MS)检测熏鱼中苯并(a)芘残留的方法。实验表明,样品经100℃的亚临界水提取5 min后,将目标物转移至环己烷-乙酸乙酯(1∶1,V/V)中,经凝胶渗透色谱(GPC)净化,Rtx-5MS毛细管气相色谱柱分离,在选择离子监测(SIM)模式下检测。目标物在0~100 ng/mL范围内线性关系良好,相关系数大于0.9999,其定量限为2.5 ng/g,检出限为1 ng/g。烟熏鱼基质中添加2.5、5和10 ng/g三个水平的标准品时,苯并(a)芘的回收率为74.89%~114.01%,相对标准偏差(RSD)为7.95%~10.56%(n=8)。该方法的灵敏度良好、准确度和精密度均符合分析要求,适用于烟熏鱼中苯并(a)芘残留的检测。
A method for detecting benzo (a) pyrene residues in smoked fish by subcritical water extraction (SCWE) and gas chromatography-mass spectrometry (GC-MS) was established. Experiments show that after the sample is extracted with subcritical water at 100 ℃ for 5 min, the target is transferred to cyclohexane-ethyl acetate (1: 1, V / V) and purified by gel permeation chromatography (GPC) -5 MS capillary gas chromatographic separation, detection in selected ion monitoring (SIM) mode. The linearity of the target ranged from 0 ng / mL to 100 ng / mL with a correlation coefficient greater than 0.9999 with a limit of quantification of 2.5 ng / g and a limit of detection of 1 ng / g. The recoveries of benzo (a) pyrene were 74.89% ~ 114.01% and the relative standard deviations (RSDs) were 7.95% ~ 10.56% at the three levels of 2.5, 5 and 10 ng / (n = 8). The method has good sensitivity, accuracy and precision are in line with the analysis requirements for the detection of benzo (a) pyrene residues in smoked fish.