Highly sensitive LC-MS-MS analysis of a pharmaceutical compound in human plasma using monolithic phase-based on-line extraction.

Monolithic columns have been used in recent years for fast chromatographic separation due to their high permeability and low backpressure. We have explored the potential of monolithic material as sample preparation tool in bioanalytical applications. By taking advantage of monolithic columns' online concentration capability, we have developed a highly sensitive liquid chromatography-tandem mass spectrometry assay for quantitative determination of a pharmaceutical compound in human plasma.

Bioanalytical hydrophilic interaction chromatography: recent challenges, solutions and applications.

Hydrophilic interaction chromatography (HILIC) has, in recent years, been shown to be an important supplement to reversed-phase liquid chromatography for polar analytes. HILIC, in conjunction with tandem mass spectrometry (MS/MS), has been steadily gaining acceptance in the analysis of polar compounds from complex biological matrices. This hyphenated technique offers the advantages of improved sensitivity by employing high organic content in the mobile phase, shortened sample preparation time with direct injection of the organic-solvent extracts of biological samples and the potential for ultra-fast analysis because of low-column backpressure.

Simultaneous LC-MS/MS quantitation of a highly hydrophobic pharmaceutical compound and its metabolite in urine using online monolithic phase-based extraction.

This article describes the use of monolithic material as extraction support in simultaneous LC-MS/MS quantitation of a highly hydrophobic pharmaceutical compound and its hydroxylated metabolite in urinary matrix. DMSO was added to urine samples to aid the solubilization of analytes during storage and transfer. Samples were then diluted and injected onto an online extraction system for high-throughput analysis in an automated fashion.

Recent advances in high-throughput quantitative bioanalysis by LC-MS/MS.

Liquid chromatography linked to tandem mass spectrometry (LC-MS/MS) has played an important role in pharmacokinetics and metabolism studies at various drug development stages since its introduction to the pharmaceutical industry. This article reviews the most recent advances in sample preparation, separation, and the mass spectrometric aspects of high-throughput quantitative bioanalysis of drug and metabolites in biological matrices. Newly introduced techniques such as ultra-performance liquid chromatography with small particles (sub-2 microm) and monolithic chromatography offer improvements in speed, resolution and sensitivity compared to conventional chromatographic techniques.

A monolithic-phase based on-line extraction approach for determination of pharmaceutical components in human plasma by HPLC-MS/MS and a comparison with liquid-liquid extraction.

An automated procedure using monolithic-phase based on-line extraction is described for pharmaceutical component analysis in plasma by LC-MS/MS. In this approach, a short monolithic C(18) 4.6 mm x 10 mm cartridge is used for high flow extraction at 4 mL/min.