Casas Ferreira Ana María, Moreno Cordero Bernardo, Pérez Pavón José Luis
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Feb 1;1043:74-80. doi: 10.1016/j.jchromb.2016.07.052. Epub 2016 Jul 30.
Sometimes it is not necessary to separate the individual compounds of a sample to resolve an analytical problem, it is enough to obtain a signal profile of the sample formed by all the components integrating it. Within this strategy, electronic noses based on the direct coupling of a headspace sampler with a mass spectrometer (HS-MS) have been proposed. Nevertheless, this coupling is not suitable for the analysis of non-volatile compounds. In order to propose an alternative to HS-MS determinations for non-volatile compounds, here we present the first 'proof of concept' use of the direct coupling of microextraction by packed sorbents (MEPS) to a mass spectrometer device using an electron ionization (EI) and a single quadrupole as ionization source and analyzer, respectively. As target compounds, a set of analytes with different physic-chemical properties were evaluated (2-ethyl-1-hexanol, styrene, 2-heptanone, among others). The use of MEPS extraction present many advantages, such as it is fast, simple, easy to automate and requires small volumes of sample and organic solvents. Moreover, MEPS cartridges are re-usable as samples can be extracted more than 100 times using the same syringe. In order to introduce into the system all the elution volume from the MEPS extraction, a programmable temperature vaporizer (PTV) is proposed as the injector device. Results obtained with the proposed methodology (MEPS-PTV/MS) were compared with the ones obtained based on the separative scheme, i.e. using gas chromatography separation (MEPS-PTV-GC/MS), and both methods provided similar results. Limits of detection were found to be between 3.26 and 146.6μgL in the non-separative scheme and between 0.02 and 1.72μgL when the separative methodology was used. Repeatability and reproducibility were evaluated with values below 17% in all cases.
有时,为了解决分析问题,不必分离样品中的各个化合物,获得由所有组分积分形成的样品信号谱就足够了。在这种策略下,有人提出了基于顶空进样器与质谱仪直接耦合(HS-MS)的电子鼻。然而,这种耦合不适用于分析非挥发性化合物。为了提出一种替代HS-MS测定非挥发性化合物的方法,在此我们展示了首次将填充吸附剂微萃取(MEPS)与质谱仪直接耦合的“概念验证”应用,分别使用电子电离(EI)和单四极杆作为电离源和分析器。作为目标化合物,评估了一组具有不同物理化学性质的分析物(2-乙基-1-己醇、苯乙烯、2-庚酮等)。MEPS萃取的使用具有许多优点,例如快速、简单、易于自动化,并且需要少量的样品和有机溶剂。此外,MEPS小柱可重复使用,因为使用同一注射器可以对样品进行100多次萃取。为了将MEPS萃取的所有洗脱体积引入系统,建议使用可编程温度汽化器(PTV)作为进样装置。将所提出方法(MEPS-PTV/MS)获得的结果与基于分离方案获得的结果进行了比较,即使用气相色谱分离(MEPS-PTV-GC/MS),两种方法提供了相似的结果。在非分离方案中,检测限在3.26至146.6μg/L之间,而使用分离方法时检测限在0.02至1.72μg/L之间。在所有情况下,重复性和再现性的评估值均低于17%。