多管漩涡混合-气相色谱-三重四极杆质谱测定油茶籽中18种多氯联苯

通过比较不同吸附剂的净化效果,建立了油茶籽中18种多氯联苯(PCBs)的气相色谱-三重四极杆质谱(GCQQQ-MS/MS)检测方法。油茶籽样品用乙腈提取,加氯化钠盐析,离心分层后提取液加无水硫酸镁、C18、N-丙基二乙胺(PSA)和多壁碳纳米管(NANO)进行多管漩涡振荡分散固相净化,GC-QQQ-MS/MS多反应监测(MRM)模式进行检测。结果表明,油茶籽中18种多氯联苯具有良好的线性关系,检出限为5μg/kg,平均回收率为109.2%,相对标准偏差为2.9%~6.2%(n=3)。方法应用于3个油茶主产省份油茶籽监测,48个油茶籽样品中18种多氯联苯均未检出。

Determination of 18 polychlorinated biphenyls in camellia seeds by multiple vortex and gas chromatography-triple quadrupole mass spectrometry

A method based on the cleaning effects of different sorbents and gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS/MS) was developed for the determination of 18 polychlorinated biphenyls (PCBs) in camellia seeds. The camellia seeds were extracted with acetonitrile, salted out with sodium chloride, then cleaned-up by QuEChERS with anhydrous MgSO₄, C18, primary secondary amine (PSA), and multi walled carbon nanotubes (NANO) using multiple vortex after the centrifugal separation, and finally analyzed by GC-QQQ-MS/MS in multiple reaction monitoring mode via positive electrospray ionization. All the 18 PCBs could be completely separated with an excellent linear relationship. The limits of detection for the 18 PCBs were 5 μg/kg. For all the samples, the mean spiked recoveries was 109.2% with relative standard deviations (RSDs) of 2.9%-6.2% (n=3). The extraction, purification and analytical methods were developed and assessed. The method was successfully applied to the 48 samples from three main producing provinces of camellia seeds. All the 18 PCBs were not detected from the 48 samples.