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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。
By comparing the purifying effects of different adsorbents, a gas chromatography-triple quadrupole mass spectrometry (GCQQQ-MS / MS) method for the determination of 18 polychlorinated biphenyls (PCBs) in camellia seed was established. The samples of Camellia oleifera were extracted with acetonitrile, salted with sodium chloride, centrifuged and the extracts were extracted with anhydrous magnesium sulfate, C18, N-propyl diethylamine (PSA) and multi-walled carbon nanotubes (NANO) Vortex and disperse solid phase purification, GC-QQQ-MS / MS multiple reaction monitoring (MRM) mode. The results showed that 18 kinds of polychlorinated biphenyls in Camellia oleifera seeds had a good linear relationship. The detection limit was 5μg / kg, the average recovery was 109.2% and the relative standard deviation was 2.9% -6.2% (n = 3). The method was applied to the monitoring of Camellia oleifera seeds in three main producing provinces of Camellia oleracea, while 18 of the 48 varieties of Camellia oleifera seeds were not detected.