Iakovides Minas, Sciare Jean, Mihalopoulos Nikos
Climate and Atmosphere Research Center (CARE-C), The Cyprus Institute, 20 Konstantinou Kavafi Str., Aglantzia 2121, Cyprus.
Chemistry Department, University of Crete, Heraklion Crete 71003, Greece.
MethodsX. 2023 May 17;10:102224. doi: 10.1016/j.mex.2023.102224. eCollection 2023.
We present a simple, selective and sensitive analytical method to quantitatively determine a wide range of halogenated persistent organic pollutants and molecular tracers in atmospheric samples. Identification and quantification was carried out by high-resolution gas chromatography, hyphenated with low-resolution mass spectrometry operating in electron impact (EI) and electron capture negative ionization (ECNI) mode. Optimization on a number of instrumental parameters was conducted to obtain ultra-trace detection limits, in the range of few fg/m for organohalogen compounds. Repeatability and reproducibility of the method was thoroughly evaluated. The analysis was validated with standard reference materials and successfully applied to actual atmospheric samples. The proposed multi-residue method provides a precise, affordable and practical procedure of sample analysis for environmental research laboratories with conventional instrumentation on a routine basis.•A simple combination of alumina, florisil and silica gel adsorbents was applied to sufficiently isolate polychlorinated biphenyls, organochlorine pesticides, polycyclic aromatic hydrocarbons, long chain -alkanes, hopanes and steranes.•Full elution was achieved in two successive fractions, using small volumes of -hexane and -hexane/dichloromethane to recover all target substances.•To maximize analytical response, optimization was applied for three operating parameters in ECNI mode: i) ion source temperature; ii) emission current; and iii) electron energy.
我们提出了一种简单、选择性强且灵敏的分析方法,用于定量测定大气样品中多种卤代持久性有机污染物和分子示踪剂。通过高分辨率气相色谱与在电子轰击(EI)和电子捕获负电离(ECNI)模式下运行的低分辨率质谱联用进行鉴定和定量。对多个仪器参数进行了优化,以获得超低的检测限,有机卤素化合物的检测限在几飞克/立方米范围内。对该方法的重复性和再现性进行了全面评估。用标准参考物质对分析进行了验证,并成功应用于实际大气样品。所提出的多残留方法为环境研究实验室提供了一种精确、经济且实用的样品分析程序,可在常规基础上使用常规仪器进行分析。
• 应用氧化铝、弗罗里硅土和硅胶吸附剂的简单组合,充分分离多氯联苯、有机氯农药、多环芳烃、长链烷烃、藿烷和甾烷。
• 使用少量正己烷和正己烷/二氯甲烷在两个连续馏分中实现完全洗脱,以回收所有目标物质。
• 为了使分析响应最大化,在ECNI模式下对三个操作参数进行了优化:i)离子源温度;ii)发射电流;iii)电子能量。