Detection and analysis of drugs-of-abuse in biological fluids are the essential tasks for the law enforcement, forensic toxicology, doping research and social health. In this work, we developed a surface-ionization mass spectrometry method for direct detection of trace amount of morphine spiked in blank urine. The mass-spectrometric analysis of spiked samples was carried out without preliminary extraction and chromatographic separation. It was found out that the major fragment ions at m/z 144, 146 could be served as indicator lines of morphine spiked in blank urine. Limit of detection of morphine spiked in blank urine was 100 pg (50 ng/ml), and a linear range of calibration curve was more than two orders of magnitude. The spiked samples were also analyzed by gas chromatography–mass spectrometry without preliminary extraction and derivatization procedures. No morphine was found in the spiked samples. The experimental data show that the high selectivity of the surface ionization can be allowed to direct analysis of morphine spiked in blank urine without its preliminary extraction and chromatographic separation.
This paper demonstrates direct detection of stimulants such as amphetamine, methamphetamine and cocaine spiked with untreated urine and a real world sample using surface ionization mass spectrometry. Spiked samples were analyzed without preliminary chromatographic separation and extraction procedure using the developed method. Moreover, in order to check the analytical capabilities of the method non-extracted real world sample was analyzed. After liquid–liquid extraction, the same sample was analyzed using the method for comparative study. Limit of detection of spiked samples was in the range of 10 pg (10 ng/ml) to 100 pg (100 ng/ml). Linear ranges of samples were two orders of magnitude or more than two orders of magnitude. It was revealed these spiked samples and real world sample can be analyzed without preliminary chromatographic separation and preliminary extraction procedure due to high selectivity of the method and the presence of the indicator lines of studied analytes in the mass spectra. The surface ionization mass spectrometry data was attested by the GC/MS analysis of these samples.
A technique for the express analysis of the products of technological processes is described, which was developed using the Raman spectroscopy method. The analysis of the Raman spectra includes the interpretation of the spectral bands, taking into account the values of the characteristic frequencies of the vibrational spectra of organic compounds, as well as the determination of the integral intensities of the corresponding spectral ranges. By example of the real time control procedure for the technological process of monosilane synthesis, the express analysis of tetraethoxysilane, which is a by-product of this technological process, is carried out. Significant advantages of using the express analysis method are demonstrated, which provide control over the normal course of the technological process and obtaining results that allow making adjustments
to the process flow diagram in order to optimize it.
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