Continuous fraction collection of gas chromatographic separations with parallel mass spectrometric detection applied to cell-based bioactivity analysis

Abstract

We describe the development and evaluation of a GC-MS fractionation platform that combines high-resolution fraction collection of full chromatograms with parallel MS detection. A y-split at the column divides the effluent towards the MS detector and towards an inverted y-piece where vaporized trap solvent is infused. The latter flow is directed outside the GC oven allowing subsequent condensation and stepwise collection of liquid fractions with trapped analytes on a 384-well plate. For study and optimization of the effluent split ratio, restriction capillaries of different lengths and diameters were evaluated. For a wide range of settings, local pressures were monitored during fractionation to assess the influence of MS vacuum and trap solvent infusion on the GC system stability. The platform performance was evaluated by GC-MS analysis and continuous fractionation of an n-alkane mixture followed by GC analysis of each fraction. Comparison of the on-line recorded and fraction-reconstructed chromatogram showed the GC separation is maintained during fractionation. Multiple fractionation cycles of the n-alkane sample on the same 384-well plate yielded a reconstructed chromatogram which was highly similar to that of a single analysis, demonstrating the high repeatability. The applicability of the GC-MS-fractionation platform for bioactivity screening was investigated by applying the AR-Ecoscreen reporter gene bioassay on fractions obtained after analysis of standard solutions and dust samples containing the anti-androgenic compounds vinclozolin and p,p'-DDE.

Effect-Directed Analysis of Ah Receptor-Mediated Potencies in Microplastics Deployed in a Remote Tropical Marine Environment

“…A GC fractionation platform with parallel MS detection, as described by Jonker et al (2017), was used for fractionation of pooled plastic samples. Prior to fractionation of real samples, the platform was evaluated for its performance by injection and qualitative analysis of five individual standards, and a mixture of 134 known compounds, including PAHs (5 ng/µL), PCBs (20-40 pg/µL), PCDD/Fs (20-100 pg/µL), PBDEs (20 pg/µL), and pesticides (20 pg/µL).…”

“…In general, liquid chromatography (LC) is used for fractionation of samples in EDA studies (Lubcke-von Varel et al, 2008;Weiss et al, 2009;Grung et al, 2011), but gas chromatography (GC) is the preferred separation technique for analysis of non-polar organic pollutants in environmental samples (Poster et al, 2006;Tombesi et al, 2017;Bjurlid et al, 2018). In recent years, a new GC-based fractionation platform with a post-column introduction of a trap solvent for fraction collection has been developed (Pieke et al, 2013;Jonker et al, 2016Jonker et al, , 2017. This platform allows for fractionation during the entire time of a GC run, thus covering a complete chromatogram.…”

“…This platform allows for fractionation during the entire time of a GC run, thus covering a complete chromatogram. Recently, the GC fractionation platform has been coupled to mass spectrometric (MS) detection for parallel analysis of compounds, and was successfully evaluated for the fractionation of a mixture of nalkanes (C 7 -C 30 ), and a mixture of two pesticides, vinclozolin and p,p'-DDE (Jonker et al, 2017).…”

Effect-directed analysis in environment research: current status and future challenges

“…样品的自动收集需要 引入自动化的分离制备装置, 收集装置应搭载玻璃 瓶、反应管、96孔甚至384孔板 [114,115] 等通用规格的批 处理容器. 除根据模式化合物保留时间进行收集外, 也 可基于特定时间间隔或特定体积等参数的分离制备策 略 [90] , 将各组分体积控制在微升剂量 [116] 或毫升剂 量 [75] .…”

Evaluation of the presence of potential hazardous substances from plastic and textile fibre recycling

“…receptor activity assay Jonker et al (2017). applied gas chromatographic (GC) fractionation of volatiles.…”