A method using supercritical fluid extraction (SFE) and gas chromatography (GC) mass spectrometry (MS) was established to analyze hexabromocyclododecane (HBCD), a brominated flame retardant, in soil. The HBCD spiked in simulated soil was extracted by SFE with optimized operating parameters and GC-MS/LC-MS was employed to detect the target analyte. The experimental results indicated that the optimum extraction conditions were 50 °C, 25 MPa, and 6 min static and 18 min dynamic extraction with 20% (v/v) modified ethanol–2% Triton X-114. The highest extraction efficiency of HBCD with optimal parameters could reach 98.9%. The differences among Soxhlet extraction, ultrasonic-assisted extraction and SFE were investigated. In comparison with other extraction methods, SFE could not only improve the extraction efficiency and shorten the extraction time but could also easily remove the extracted impurities. Furthermore, the established analytical method was applied to detect HBCD in field soils and the average concentration in real soil samples was 0.96 mg kg⁻¹. This work provides an efficient, rapid and easy way to conduct the extraction and detection of HBCD in soil.

中文翻译：

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超临界流体萃取-气相色谱质谱法测定土壤中的六溴环十二烷

建立了一种使用超临界流体萃取（SFE）和气相色谱（GC）质谱（MS）的方法来分析土壤中的溴代阻燃剂六溴环十二烷（HBCD）。通过SFE用优化的操作参数提取加标在模拟土壤中的六溴环十二烷，并使用GC-MS / LC-MS检测目标分析物。实验结果表明，最佳萃取条件为50°C，25 MPa，6分钟静态萃取和18分钟动态萃取，采用20％（v / v）改性乙醇–2％Triton X-114。最佳参数对六溴环十二烷的提取效率最高，可达98.9％。研究了索氏提取，超声辅助提取和超临界流体萃取之间的差异。与其他提取方法相比，SFE不仅可以提高萃取效率并缩短萃取时间，而且还可以轻松去除萃取出的杂质。此外，采用建立的分析方法检测田间土壤中的六溴环十二烷，实际土壤样品中的平均浓度为0.96 mg kg^-1。这项工作为在土壤中进行六溴环十二烷的提取和检测提供了一种有效，快速和简便的方法。