Triñanes Sara, Pena Ma Teresa, Casais Ma Carmen, Mejuto Ma Carmen
Departamento Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain.
Departamento Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain.
Talanta. 2015 Jan;132:433-42. doi: 10.1016/j.talanta.2014.09.044. Epub 2014 Oct 7.
A new straightforward and inexpensive sample screening method for both EPA and EU priority polycyclic aromatic hydrocarbons (PAHs) in water has been developed. The method is based on combined direct immersion and headspace (DIHS) sorptive extraction, using low-cost disposable material, coupled to ultraperformance liquid chromatography with fluorescence and UV detection (UPLC-FD-UV). Extraction parameters, such as the sampling mode, extraction time and ionic strength were investigated in detail and optimized. Under optimized conditions, water samples (16 mL) were concentrated in silicone disks by headspace (HS) and direct immersion (DI) modes simultaneously, at room temperature for 9h for the majority of the 24 studied compounds. Ultrasound-assisted desorption of extracted analytes in acetonitrile was carried out also at room temperature. The optimized chromatographic method provided a good linearity (R≥0.9991) and a broad linear range for all studied PAHs. The proposed analytical procedure exhibited a good precision level with relative standard deviations below 15% for all analytes. Quantification limits between 0.7 and 2.3 µg L(-1) and 0.16 and 3.90 ng L(-1) were obtained for compounds analyzed by UV (acenaphtylene, cyclopenta[c,d]pyrene and benzo[j]fluoranthene) and fluorescence, respectively. Finally, the proposed method was applied to the determination of PAHs in different real tap, river and wastewater samples.
已开发出一种用于水中美国环保署（EPA）和欧盟优先控制的多环芳烃（PAHs）的新型直接且低成本的样品筛查方法。该方法基于直接浸入与顶空（DIHS）相结合的吸附萃取，使用低成本一次性材料，与配有荧光和紫外检测的超高效液相色谱（UPLC-FD-UV）联用。详细研究并优化了萃取参数，如采样模式、萃取时间和离子强度。在优化条件下，对于大多数研究的24种化合物，16 mL水样在室温下通过顶空（HS）和直接浸入（DI）模式同时在硅胶盘上浓缩9小时。萃取的分析物在室温下也通过超声辅助在乙腈中解吸。优化的色谱方法对所有研究的PAHs具有良好的线性（R≥0.9991）和较宽的线性范围。所提出的分析程序对所有分析物具有良好的精密度水平，相对标准偏差低于15%。通过紫外检测（苊烯、环戊并[c,d]芘和苯并[j]荧蒽）和荧光分析的化合物的定量限分别为0.7至2.3 μg L⁻¹和0.16至3.90 ng L⁻¹。最后，将所提出的方法应用于不同实际自来水、河水和废水样品中PAHs的测定。
