本文建立了鱼肉中16种多环芳烃的气相色谱-三重四级杆串联质谱（GC-QqQ-MS/MS）的检测方法。样品通过正己烷/二氯甲烷(1/1，V/V)超声波提取，经弗罗里硅土柱净化后，采用TR-5MS毛细管柱分离，以电子轰击（EI）电离、选择反应检测模式（SRM）检测。讨论了洗脱溶剂对净化效果的影响，以及基质效应对各种多环芳烃测定的影响。通过基质匹配标准曲线进行定量，16种多环芳烃在0.4 μg/kg到50 μg/kg范围内相性关系良好，线性相关系数为0.9865~0.9999。方法检出限从0.024 μg/kg到0.06 μg/kg，方法的定量限从0.08 μg/kg到0.2 μg/kg。16种多环芳烃在5、10、50 μg/kg加标水平下的回收率为68.5%到106.3%，相对标准偏差为0.4%到17.8%，对常见的鱼类样品进行测定，结果令人满意。

A new GC-QqQ–MS/MS method was developed to determine the polycyclic aromatic hydrocarbons (PAHs) in fish. In this method, the samples were pretreated by ultrasonic extraction with hexane/dichloromethane and purified with hexane/acetone on florisil column, and then analyzed on a TR-5MS column. PAHs can be detected in the modes of electron impact ionization and selective reaction monitoring. The calibration curves had good linearity within 0.4~50 μg/kg for each pesticide (0.9999＞R＞0.9865). The limits of the detection ranged from 0.024 μg/kg to 0.06 μg/kg and the limits of quantitation ranged from 0.08 μg/kg to 0.2 μg/kg. The recoveries of PAHs varied from 68.5% to 106.3% with the relative standard deviations of 0.3~17.8% at the spiked levels 5, 10 and 50 μg/kg. It was satisfied with successfully determination of fish samples by this analytical approach.

河南省基础前沿与技术研究计划项目（122300410428）