Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huai River Water Environmental Pollution and Control, Ministry of Education, School of Environment, Henan Normal University, Xinxiang, 453007, PR China; Key Laboratory of Green Chemical Media and Reactions, Ministry of Education, Collaborative Innovation Center of Henan Province for Green Manufacturing of Fine Chemicals, Xinlian College, School of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang, 453007, PR China.
Key Laboratory of Green Chemical Media and Reactions, Ministry of Education, Collaborative Innovation Center of Henan Province for Green Manufacturing of Fine Chemicals, Xinlian College, School of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang, 453007, PR China.
Anal Chim Acta. 2020 Jun 8;1115:7-15. doi: 10.1016/j.aca.2020.04.019. Epub 2020 Apr 12.
Solvent-free analysis of organic pollutants from a complex matrix has attracted significant attention. In this work, we designed and fabricated a facile cooling-assisted solid-phase microextraction device (CA-SPME) that could be used for the solvent-free extraction of volatile and semivolatile compounds from a complex matrix using a commercial SPME probe. Determination of polycyclic aromatic hydrocarbons (PAHs) from soil samples was carried out to evaluate the performance of the designed CA-SPME device. The effects of heating temperature, cooling temperature, extraction time, and moisture content in soil on extraction efficiency were investigated. To enhance the extraction efficiency of the targeted analytes, the matrix solid-phase dispersion technique (MSPD) by grinding soil with silica gels was applied. The results showed that grinding with silica gels promoted the release of PAHs from the soil matrix to the headspace by disrupting the matrix structure, which then facilitated the extraction efficiency. Under optimized conditions, for all of the targeted PAHs, the method exhibited good linearity (40-4000 ng g) with regression coefficients (R) ranging from 0.9586 to 0.9964. The limits of detection and limits of quantification ranged from 4.2 to 8.5 ng g and 14.0-28.5 ng g, respectively. Relative standard deviations corresponding to the analysis of spiked soil samples (n = 5) were 8.1-13.4%. The solvent-free analysis of the certified soil sample using the proposed method demonstrated satisfactory results.
无溶剂分析复杂基质中的有机污染物引起了广泛关注。在这项工作中，我们设计并制造了一种简单的冷却辅助固相微萃取装置（CA-SPME），该装置可用于使用商业 SPME 探头从复杂基质中无溶剂提取挥发性和半挥发性化合物。我们通过测定土壤样品中的多环芳烃（PAHs）来评估所设计的 CA-SPME 装置的性能。考察了加热温度、冷却温度、萃取时间以及土壤中的水分含量对萃取效率的影响。为了提高目标分析物的萃取效率，我们采用了基质固相分散技术（MSPD），通过用硅胶研磨土壤来实现。结果表明，用硅胶研磨可以通过破坏基质结构来促进 PAHs 从土壤基质中释放到顶空，从而提高萃取效率。在优化条件下，对于所有目标 PAHs，该方法均表现出良好的线性关系（40-4000 ng g），相关系数（R）范围为 0.9586-0.9964。检出限和定量限范围分别为 4.2-8.5 ng g 和 14.0-28.5 ng g。对于加标土壤样品的分析，相对标准偏差为 8.1-13.4%（n=5）。使用该方法对认证土壤样品进行无溶剂分析，结果令人满意。
