分析科学学报

建立了静态顶空-同位素内标-气相色谱/质谱联用法测定工业清洗剂中8种多环芳烃(PAHs),包括萘、苊烯、苊、芴、菲、蒽、苯并[a]蒽和■。样品经乙腈分散溶解,加入苊-D₁₀、菲-D₁₀和■-D₁₂混合内标溶液,超声提取后取100μL上清液进行顶空分析。顶空进样有效避免了基质干扰,提高了方法选择性。乙腈作为分散剂对8种PAHs具有良好的顶空释放效果。优化后的顶空平衡条件为150℃、15min。实验结果表明,8种PAHs在0.50～20.0mg·L^-1范围内线性关系良好,相关系数(R)²>0.997,方法定量限为3.7～5.6mg·kg^-1;在10、20、100mg·kg^-13个加标水平下,回收率范围为73.6%～125.9%,相对标准偏差为1.5%～13.9%。实验对20款市售工业清洗剂进行筛查,其中3款检出萘,最高含量达2.7×10~3mg·kg^-1。所建立方法可为工业清洗剂中PAHs检测提供高效、准确的技术方案。

A static headspace-isotope internal standard-gas chromatography-mass spectrometry method was established for the determination of eight polycyclic aromatic hydrocarbons(PAHs) in industrial cleaning agents.The target analytes included naphthalene,acenaphthylene,acenaphthene,fluorene,phenanthrene,anthracene,benz[a]Anthracene,and chrysene.Samples were dispersed in acetonitrile,spiked with a mixed internal standard(acenaphthene-D₁₀,phenanthrene-D₁₀,and chrysene-D₁₂),and subjected to ultrasonic extraction.A 100 μL aliquot of the supernatant was analyzed via headspace injection.The headspace sampling effectively eliminated matrix interference and enhanced method selectivity.Acetonitrile demonstrated efficient headspace release for all eight PAHs.Optimized headspace equilibrium conditions were 150℃ for 15 min.Calibration curves showed good linearity(R²>0.997) in the concentration range of 0.50-20.0 mg·L^-1.Method quantification limits ranged from 3.7 to 5.6 mg·kg^-1.Recoveries at three spiked levels(10,20,and 100 mg·kg^-1) were 73.6%-125.9%,with relative standard deviation(RSD) of 1.5%-13.9%.Screening of 20 commercial industrial cleaning agents revealed naphthalene in three products,with a maximum concentration of 2.7×10³ mg·kg^-1.This method provides an efficient and accurate technical solution for PAHs detection in industrial cleaning agents.