Pérez Pavón José Luis, del Nogal Sánchez Miguel, Fernández Laespada María Esther, Moreno Cordero Bernardo
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
J Chromatogr A. 2008 Aug 22;1202(2):196-202. doi: 10.1016/j.chroma.2008.07.024. Epub 2008 Jul 12.
A sensitive method is presented for the fast analysis of three aromatic and six polycyclic aromatic hydrocarbons (biphenyl, 3-methylbiphenyl, 4-methylbiphenyl, fluorene, phenanthrene, fluoranthene, pyrene, 1,2-benz(a)anthracene and chrysene) in gasoline samples. The applicability of a GC device equipped with a programmable temperature vaporizer (PTV) and an MS detector is explored. Additionally, a modular accelerated column heater (MACH) was used to control the temperature of the capillary gas chromatography column. This module can be heated and cooled very rapidly, making total analysis cycle times very short. The proposed method does not require any previous analyte extraction and preconcentration step, as in most methods described to date. Sample preparation is reduced to simply diluting the gasoline samples in methanol. This reduces the experimental errors associated with this step of the analytical process. By using sampling injection in the solvent vent mode, and through choice of a suitable temperature, the lightest major components of the gasoline were removed. Moreover, use of a liner packed with Tenax-TA allowed the compounds of interest to be retained during the process. This working strategy could be extended to other groups of compounds through the choice of different venting temperatures. In this way, a large part of the gasoline components are eliminated, the life of the liner is prolonged, and it is possible to inject sample volumes that will not saturate the chromatographic column. The limits of detection ranged from 0.61 microg/L (pyrene) to 6.1 microg/L (biphenyl), and precision (measured as the relative standard deviation) was equal to or lower than 7.3%. The method was applied to the determination of analytes in gasoline samples and the results obtained can be considered highly satisfactory.
本文提出了一种灵敏的方法,用于快速分析汽油样品中的三种芳香烃和六种多环芳烃(联苯、3-甲基联苯、4-甲基联苯、芴、菲、荧蒽、芘、1,2-苯并(a)蒽和 Chrysene)。探讨了配备可编程温度汽化器(PTV)和质谱检测器的气相色谱仪的适用性。此外,还使用了模块化加速柱加热器(MACH)来控制毛细管气相色谱柱的温度。该模块可以非常快速地加热和冷却,使总分析周期时间非常短。与迄今为止描述的大多数方法不同,所提出的方法不需要任何先前的分析物萃取和预浓缩步骤。样品制备简化为只需将汽油样品用甲醇稀释。这减少了与分析过程这一步骤相关的实验误差。通过在溶剂放空模式下进行采样进样,并通过选择合适的温度,去除了汽油中最轻的主要成分。此外,使用填充有Tenax-TA的衬管可使目标化合物在该过程中得以保留。通过选择不同的放空温度,这种工作策略可以扩展到其他化合物组。通过这种方式,消除了大部分汽油成分,延长了衬管的使用寿命,并且可以进样不会使色谱柱饱和的样品体积。检测限范围为0.61μg/L(芘)至6.1μg/L(联苯),精密度(以相对标准偏差衡量)等于或低于7.3%。该方法应用于汽油样品中分析物的测定,所得结果可认为非常令人满意。