Richter Pablo, Jiménez Marcela, Salazar Ricardo, Maricán Adolfo
Departamento de Química Inorgánica y Analítica, Facultad de Ciencias Químicas y Farmacéuticas, Universidad de Chile, Olivos 1007, Independencia, P.O. Box 233, Santiago, Chile.
J Chromatogr A. 2006 Nov 3;1132(1-2):15-20. doi: 10.1016/j.chroma.2006.07.013. Epub 2006 Sep 18.
In the present work the efficiency of extraction of aliphatic diesel range organics (DROs) and polycyclic aromatic hydrocarbons (PAHs) from soil was assessed by using dynamic modes of pressurized solvent extraction (PSE), and ultrasound-assisted pressurized solvent extraction (US-PSE). Optimization studies were carried out using a blank soil (Non-Polluted Soil#1, CLN-1, RTC) and a real soil which was previously spiked with the analyte mixture and aged for 90 days. A laboratory-made manifold with controlled temperature and pressure was used to carry out the leaching processes. The extraction cell was inserted into an oven for PSE and into an ultrasound bath for US-PSE. The following variables were studied in each case, keeping the pressure at about 1800 psi: extraction temperature, time of static and dynamic extraction and solvent flow rate. In addition, the time of ultrasound application was also studied in US-PSE. For PSE with dichloromethane (DCM) the recoveries were about 90-95% for both the families of analytes, using extraction times of 20 min. Analyte extraction was quantitative by using US-PSE with DCM for 10 min. In all cases, after the extraction process, the analytes were determined by GC-MS. Application of the method to a natural contaminated sample suggests that either the extraction time used in US-PSE should be increased to 20 min or the solvent (DCM) should be replaced by a mixture of DCM:acetone (1:1), to reach comparability with Soxhlet extraction.
在本研究中,采用加压溶剂萃取(PSE)的动态模式以及超声辅助加压溶剂萃取(US-PSE),评估了从土壤中萃取脂肪族柴油范围有机物(DROs)和多环芳烃(PAHs)的效率。使用空白土壤(无污染土壤#1,CLN-1,RTC)和预先添加分析物混合物并老化90天的实际土壤进行了优化研究。使用一个具有可控温度和压力的实验室自制歧管进行浸出过程。将萃取池插入用于PSE的烘箱中以及用于US-PSE的超声浴中。在每种情况下,保持压力约为1800 psi,研究以下变量:萃取温度、静态和动态萃取时间以及溶剂流速。此外,还研究了US-PSE中超声施加时间。对于使用二氯甲烷(DCM)的PSE,两种分析物家族的回收率在萃取时间为20分钟时约为90 - 95%。使用DCM进行10分钟的US-PSE可实现分析物的定量萃取。在所有情况下,萃取过程结束后,通过气相色谱 - 质谱联用仪(GC-MS)测定分析物。将该方法应用于天然污染样品表明,要么将US-PSE中使用的萃取时间增加到20分钟,要么将溶剂(DCM)替换为DCM与丙酮(1:1)的混合物,以达到与索氏萃取相当的效果。