气相色谱-三重四极杆串联质谱法测定海产品中18种多环芳烃

目的 建立海产品中18种多环芳烃化合物(PAHs)的气相色谱-三重四极杆串联质谱(GC-MS/MS)检测方法。方法 海产品冻干粉末用环己烷-乙酸乙酯(1∶1,v/v)为溶剂快速溶剂萃取,提取液经凝胶渗透色谱法净化后,用气相色谱-串联质谱法(GC-MS/MS)测定。结果 被测物以DB-5MS毛细管柱分离、MS/MS选择反应监测模式(SRM)检测,在1.0μg/L~100μg/L范围内,相关系数>0.999,方法检出限(S/n=3)为0.074μg/kg~0.18μg/kg(干重),相对标准偏差(RSD)为1.1%~6.8%,加标回收率为71.2%~110.6%,相对标准偏差(RSD)为3.4%~13.6%(n=6)。结论 方法准确、灵敏、重复性好,满足海产品中18种PAHs检测的要求。

Determination of 18 polycyclic aromatic hydrocarbons in seafood by gas chromatography-triple quadrupole tandem mass spectrometry

Objective To establish a method for determinating 18 polycyclic aromatic hydrocarbons (PAHs) in seafood by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS).Methods The PAHs in freezing dried seafood powder were extracted by a pressurized solvent extraction (PSE) with cyclohexane-ethyl acetate (1∶1,v/v) serving as extractant and the extract was determined by the gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) after purified by the gel permeation chromatography (GPC).Results After separated with DB-5MS column and detected with SRM mode of tandem mass spectrometry,the calibration curves showed good linearities for 18 PAHs in the range of 1.0 μg/L-100 μg/L with r>0.999.The detection limits (S/N=3) of 18 PAHs were between 0.074 μg/kg and 0.18 μg/kg (dry weight) with the relative standard deviations (RSDs) of 1.1 %-6.8 %.The average recoveries of 18 PAHs were from 71.2% to 110.6% with the relative standard deviations of 3.4%-13.6% (n=6).Conclusion The developed method is selective,accurate and sensitive and meets the requirements for monitoring PAHs in marine products.