吸附剂针对性净化-气相色谱-三重四极杆串联质谱测定油茶果中55种持久性有机污染物

建立了针对性净化与气相色谱-串联质谱相结合的方法，测定油茶果不同部位中16种多环芳烃、18种多氯联苯和21种有机氯共55种持久性有机污染物（POPs）。油茶籽仁、油茶外种皮和油茶壳样品采用乙腈提取，氯化钠盐析，离心分层后，分别向提取液中加入无水硫酸镁和PSA、C18、Florisil、Si、SCX、NANO Carb与Pesticarb等 7种吸附剂进行多管漩涡振荡分散固相净化比较，多反应监测模式检测。结果表明，55种持久性有机污染物在20~1 000 μg/L浓度范围内具有良好的线性关系，检出限为0.25~65.50 μg/kg，定量限为0.84~218.34 μg/kg，加标回收率为69.1%~138.2%。应用本方法检测来自湖南、江西和浙江共54份油茶的POPs，从油茶籽仁检出萘、狄氏剂、芴、毒杀芬、菲、α-六六六和苊萘嵌戊烷（4.36~566.26 μg/kg）；外种皮检出萘、芴、菲、毒杀芬、α-六六六和苊萘嵌戊烷（3.62~1 109.43 μg/kg）；油茶壳检出萘、毒杀芬、芴和菲（5.13~703.57 μg/kg）。该方法适用于油茶果不同部位持久性有机污染物的检测，对其他油料作物的POPs分析也具有一定的参考价值。

Determination of 55 Persistent Organic Pollutants in Camellia Fruits by Adsorbents Targeted Purification and Gas Chromatography-Tandem Mass Spectrometry

A method based on adsorbents targeted purification and gas chromatography-tandem mass spectrometry was developed for the determination of 55 kinds of persistent organic pollutants (POPs) including 16 kinds of polycyclic aromatic hydrocarbons, 18 kinds of polychlorinated biphenyls and 21 kinds of organic chlorines in different parts of camellia fruits. The camellia seed kernel, episperm and shell were extracted with acetonitrile, salted out with sodium chloride, then cleaned-up by QuEChERS with PSA, C18, Florisil, Si, SCX, NANO Carb and Pesticarb using multiple vortex after centrifugal separation, and finally analyzed at multiple reaction monitoring mode via positive electrospray ionization. All the 55 POPs could be completely separated with an excellent linear relationship in the concentration range of 20-1 000 μg/L. The determination limits and quantification limits of the 55 POPs were 0.25-65.50 μg/kg and 0.84-218.34 μg/kg, respectively. For all the samples, the mean spiked recoveries were 69.06%-138.15%. The extraction, purification and analysis methods were developed and assessed. The method was successfully applied to the 54 camellia fruit samples from Hunan, Jiangxi and Zhejiang provinces. Nap, dieldrin, FL, toxaphene, Phe, α-BHC and ACE were detected from 4.36 μg/kg to 566.26 μg/kg in kernels. Nap, FL, Phe, toxaphene, α-BHC and ACE were detected from 3.62 μg/kg to 1 109.43 μg/kg in episperm. Nap, toxaphene, FL and Phe were detected from 5.13 μg/kg to 703.57 μg/kg in shell. The method is not only suitable for the detection of POPs in different parts of camellia fruit, but also has certain reference value for the analysis of POPs in other oil crops.