采用连续超声辅助加压溶剂萃取和气相色谱 - 质谱联用技术测定生物固体中的多氯联苯
Determination of polychlorinated biphenyls in biosolids using continuous ultrasound-assisted pressurized solvent extraction and gas chromatography-mass spectrometry.
作者信息
Rocco Gabriela, Toledo Carla, Ahumada Inés, Sepúlveda Betsabet, Cañete Alvaro, Richter Pablo
机构信息
Departamento de Química Inorgánica y Analítica, Facultad de Ciencias Químicas y Farmacéuticas, Universidad de Chile, Casilla 233, Santiago, Chile.
出版信息
J Chromatogr A. 2008 Jun 6;1193(1-2):32-6. doi: 10.1016/j.chroma.2008.04.020. Epub 2008 Apr 16.
An efficient continuous pressurized solvent extraction (PSE) method assisted by ultrasound energy was developed for the extraction of polychlorinated biphenyls (PCBs) from biosolids. Analytes were determined in the extracts by gas chromatography-mass spectrometry in selected ion monitoring (SIM) mode. A screening-type experimental design pointing to dynamic extraction time as the only significant variable in the extraction process was carried out to optimize PCB extraction from the biosolids. Final selected conditions for PSE were extraction temperature, 50 degrees C; static extraction time, 0 min; and dynamic extraction time, 30 min. Recovery of the PSE method was 73%, which was significantly improved (103%) when PSE was assisted with 30-min ultrasound (US-PSE). Precision of the overall method, expressed as relative standard deviation, was 3.6% and the detection limit was 0.037 mg/kg. The method was applied to the determination of PCBs in biosolids from different water treatment plants from central Chile.
开发了一种高效的连续加压溶剂萃取（PSE）方法，该方法借助超声能量从生物固体中萃取多氯联苯（PCBs）。通过气相色谱 - 质谱联用仪在选择离子监测（SIM）模式下测定提取物中的分析物。进行了一种筛选型实验设计，将动态萃取时间作为萃取过程中唯一的显著变量，以优化从生物固体中萃取多氯联苯。PSE的最终选定条件为：萃取温度50℃；静态萃取时间0分钟；动态萃取时间30分钟。PSE方法的回收率为73%，当PSE辅以30分钟超声处理（US - PSE）时，回收率显著提高（103%）。以相对标准偏差表示的整个方法的精密度为3.6%，检测限为0.037 mg/kg。该方法应用于智利中部不同水处理厂生物固体中多氯联苯的测定。
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