摘要
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0.4μg/kg到50μg/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0.024μg/kg到0.06μg/kg,方法的定量限从0.08μg/kg到0.2μg/kg。16种多环芳烃在5、10、50μg/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（0.9999R0.9865）.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.
出处
《现代食品科技》
EI
CAS
北大核心
2013年第6期1395-1399,共5页
Modern Food Science and Technology
基金
河南省基础前沿与技术研究计划项目(122300410428)
关键词
气相色谱-三重四级杆串联质谱
多环芳烃
鱼肉
gas chromatography-triple quadrupole mass spectrometry
polycyclic aromatic hydrocarbons
fish
