RESUMO
A major problem limiting reproducible use of liquid extraction surface analysis (LESA) array sampling of dried surface-deposited liquid samples is the unwanted spread of extraction solvent beyond the dried sample limits, resulting in unreliable data. Here, we explore the use of the Droplet Microarray (DMA), which consists of an array of superhydrophilic spots bordered by a superhydrophobic material giving the potential to confine both the sample spot and the LESA extraction solvent in a defined area. We investigated the DMA method in comparison with a standard glass substrate using LESA analysis of a mixture of biologically relevant compounds with a wide mass range and different physicochemical properties. The optimized DMA method was subsequently applied to urine samples from a human intervention study. Relative standard deviations for the signal intensities were all reduced at least 3-fold when performing LESA-MS on the DMA surface compared with a standard glass surface. Principal component analysis revealed more tight clusters indicating improved spectral reproducibility for a human urine sample extracted from the DMA compared to glass. Lastly, in urine samples from an intervention study, more significant ions (145) were identified when using LESA-MS spectra of control and test urine extracted from the DMA. We demonstrate that DMA provides a surface-assisted LESA-MS method delivering significant improvement of the surface extraction repeatability leading to the acquisition of more robust and higher quality data. The DMA shows potential to be used for LESA-MS for controlled and reproducible surface extraction and for acquisition of high quality, qualitative data in a high-throughput manner.
Assuntos
Arginina/isolamento & purificação , Difenidramina/isolamento & purificação , Extração Líquido-Líquido , Rafinose/isolamento & purificação , Rodaminas/isolamento & purificação , Taurina/isolamento & purificação , Vitamina B 12/isolamento & purificação , Arginina/química , Arginina/urina , Difenidramina/química , Difenidramina/urina , Voluntários Saudáveis , Humanos , Interações Hidrofóbicas e Hidrofílicas , Masculino , Espectrometria de Massas , Rafinose/química , Rafinose/urina , Rodaminas/química , Rodaminas/urina , Propriedades de Superfície , Taurina/química , Taurina/urina , Vitamina B 12/química , Vitamina B 12/urinaRESUMO
The labelling of the cationic dye Rhodamine-123 with 125I is described. The biodistribution of the iodinated Rhodamine-123 has been determined at different time intervals after intravenous injection into fasted rats. It turned out that the dye is predominantly cleared by the liver and discharged into the bile. The bile acid taurocholate did not enhance the rate of excretion of 125I-Rhodamine-123.