Представлена ВЭЖХ-МС/МС-методика селективного и надежного скринингового определения кортикостероидов и диуретиков в моче человека. Процедура пробоподготовки заключается в проведении экстракции, упаривании органического экстракта в токе азота и перерастворении сухого остатка. Экстракт проанализирован методом высокоэффективной жидкостной хроматографии в сочетании с тандемной масс-спектрометрией с использованием электрораспылительной ионизации при атмосферной ионизации с регистрацией отрицательных ионов. Для всех определяемых соединений получены масс-спектры и определены характеристичные ионы, времена удерживания и пределы детектирования, при валидации процедуры проведена оценка степени подавления ионизации матрицей и извлечения аналитов из биологической жидкости человека, селективности и специфичности определения соединений.

A method is proposed for the detection and confirmation of the presence of beta-blockers and their metabolites in fivefold diluted human urine samples by ultra performance liquid chromatography coupled with electrospay ionization tandem mass spectrometry. The limits of detection for most of compounds are 5–10 ng/mL. A substantial effect of ionization suppression was observed. The determination of metabolites and glucuronides of beta-blockers without additional derivatization and extraction is described for the first time.

The objective of this study was to demonstrate the possibility to use deuterated compounds as internal standards for the quantitative analysis of morphine by gas chromatography with mass-selective detection for the purpose of doping control. The paper is focused on the problems associated with the use of deuterated morphine-D3 as the internal standard. Quantitative characteristics of the calibration dependence thus documented are presented along with uncertainty values obtained in the measurements with the use of deuterated morphine-D6. An approach to the assessment of method bias associated with the application of morphine-D6 as the deuterated internal standard is described.

Factors affecting the sensitivity and selectivity of the determination of diuretics, anabolic steroids, central nervous system stimulants, and narcotics in the analysis of human urine extracts by high-performance liquid chromatography-tandem mass spectrometry with atmospheric pressure electrospray ionization and recording of positive ions were investigated. Mass spectra were obtained for all of the test compounds; the characteristic ions, retention times, detection limits, degree of ionization suppression by the matrix, the extraction of the analytes from human biological fluids were determined for all analytes; the selectivity and specificity of determination were evaluated.