E7090, a novel fibroblast growth factor receptors inhibitor, is currently under clinical development for the treatment of patients with solid tumors. Assays for the determination of E7090 concentrations in human plasma and urine have been developed using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to evaluate pharmacokinetic profiles of E7090. E7090 and a deuterated labeled internal standard (IS) were extracted from 50 μL of plasma by protein precipitation.
View Article and Find Full Text PDFA simple and reproducible bioanalytical method for the determination of flecainide in human plasma was developed and validated using an ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) to obtain higher sensitivity than the current available methods. After simple protein precipitation, flecainide and a stable isotope-labeled internal standard (IS) were chromatographed on an Acquity UPLC BEH C18 column (2.1 × 100 mm, 1.
View Article and Find Full Text PDFA novel metal aquo-ion affinity chromatography has been developed for the analysis of basic compounds using heat-treated silica gel containing hydrated metal cations (metal aquo-ions) as the packing material. The packing materials of the metal aquo-ion affinity chromatography were prepared by the immobilization of a single metal component such as Fe(III), Al(III), Ag(I), and Ni(II) on silica gel followed by extensive heat treatment. The immobilized metals form aquo-ions to present cation-exchange ability for basic analytes and the cation-exchange ability for basic analytes depends on pKa of the immobilized metal species.
View Article and Find Full Text PDFWe examined the suppression methodology of the interaction between phosphate compounds, such as nucleotides, and the stainless steel surfaces of high-performance liquid chromatography and electrospray ionization mass spectrometry (HPLC/ESI-MS) equipment in an effort to prevent the tailing of peaks seen in HPLC chromatograms of phosphate compounds. Addition of carbonate (CO(3)(2-)) to mobile phase was highly effective in suppressing the interaction of phosphate compounds derived from a complexation between phosphate groups and metal ions that exist on a stainless steel surface in a mechanism similar to Fe(III)- and Cr(III)-immobilized metal affinity chromatography (IMAC). Addition of ammonium hydrogen carbonate to mobile phase achieved a simple and reliable HPLC/ESI-MS analysis of mono-, di-, and triphosphate compounds (six nucleotides) without peak tailing due to the interaction between stainless steel surfaces and phosphate groups.
View Article and Find Full Text PDFTo solve the problem of carry-over--a persistent chromatographic challenge for bioanalytical assays with highly sensitive detector such as a mass spectrometry (MS)--a new on-line sample pretreatment HPLC/MS system using a column-switching technique was established. This system was designed to reduce carry-over based on a hydrophobic interaction mechanism using a washing function (multi-mobile phase flow system), as well as to remove impurities on-line in a mobile phase for the pretreatment. As a result, a washing function in this system was enabled to reduce carry-over and to remove impurities in a mobile phase by automatic operation.
View Article and Find Full Text PDFThe effect of the presence of foreign salts (NaCl, aerosol OT, tetra-n-hexylammonium bromide, and CH3COONH4) on the formation of gaseous ions for electrospray (ES) and laser spray (LS) was studied in the positive and negative modes of operations. The ion signals for amino acids show sudden decrease with the concentration of foreign salts greater than 10(-5) M for both ES and LS. When the surface-active counter ions were added, the signal intensities showed a marked decrease for both ES and LS.
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