Introduction of solid-phase microextraction as a high-throughput sample preparation tool in laboratory analysis of prohibited substances

Boyacı, Ezel
Rodriguez-Lafuente, Angel
Bojko, Barbara
Pawliszyn, Janusz
A fully automated, high-throughput method based on thin-film solid-phase microextraction (SPME) and liquid chromatography-mass spectrometry was developed for simultaneous quantitative analysis of 110 doping compounds, selected from ten classes and varying in physical and chemical properties. Among four tested extraction phases, C18 blades were chosen, as they provided optimum recoveries and the lowest carryover effect. The SPME method was optimized in terms of extraction pH, ionic strength of the sample, washing solution, extraction and desorption times for analysis of urine samples. Chromatographic separation was obtained in reversed-phase model; for detection, two mass spectrometers were used: triple quadrupole and full scan orbitrap. These combinations allowed for selective analysis of targeted compounds, as well as a retrospective study for known and unknown compounds. The developed method was validated according to the Food and Drug Administration (FDA) criteria, taking into account Minimum Required Performance Level (MRPL) values required by the World Anti-Doping Agency (WADA). In addition to analysis of free substances, it was also shown that the proposed method is able to extract the glucuronated forms of the compounds. The developed assay offers fast and reliable analysis of various prohibited substances, an attractive alternative to the standard methods that are currently used in anti-doping laboratories.


Development of new synthetic methodologies for indole derivatives
Kılıklı, Ahmet Alper; Balcı, Metin; Department of Chemistry (2010)
Synthesizing nitrogen containing heterocyclic compounds is one of the leading research areas throughout the organic chemistry due to their significant activities on biological systems. Among the various biologically active molecules, indole derivatives are of prime importance on the grounds of their proven clinical roles. Objective of this study is to synthesize new indole derivatives those may contribute treatment of several diseases like their analogues via a recently developed synthetic methodology. Besi...
Optimization of ETV-ICP(TOF)MS and transient signal profiles for reducing isobaric interferences
Ertaş, Gülay (Royal Society of Chemistry (RSC), 2005-01-01)
One of the advantages of the ETV sample introduction is the ability to temporally separate analyte elements in complex mixtures by differences in their vaporization temperatures within the ETV for ICPMS. However, the broadening of the transient peaks in the transport tubing often obscures this temporal resolution. This study shows that decreasing the transport tubing diameter produces little broadening beyond that produced during aerosol production in the ETV. Maintaining such narrow peaks through the trans...
Development of sensitive analytical methods for the determination of thallium at trace levels by slotted quartz tube flame atomic absorption spectrometry
Ari, Betul; BAKIRDERE, Sezgin; Ataman, Osman Yavuz (Elsevier BV, 2020-09-01)
A simple, sensitive and economical technique is needed for the determination of thallium and this study demonstrates the different analytical strategies were developed using atomic absorption spectrometry (AAS). In order to improve the sensitivity of flame atomic absorption spectrometry (FAAS), a basic slotted quartz tube (SQT) was used for the thallium determination. In the first strategy, mixing propanol (100 mu L) and Tl standard solution (500 mu L) under the optimum conditions, namely solvent assisted S...
Novel Pt(II) complexes containing pyrrole oxime, synthesis, characterization and DNA binding studies
Altunöz Erdoğan, Deniz; Ozalp-Yaman, Seniz (Elsevier BV, 2014-05-05)
Since the discovery of anticancer activity and subsequent clinical success of cisplatin (cis-[PtCl2(NH3)(2)]), platinum-based compounds have since been widely synthesized and studied as potential chemotherapeutic agents. In this sense, three novel nuclease active Pt(II) complexes with general formula; [Pt(NH3)CI(L)] (1), [Pt(L)(2)] (2), and K[PtCl2(L)] (3) in which L is 1-H-pyrrole-2-carbaldehyde oxime were synthesized. Characterization of complexes was performed by elemental analysis, FT-IR, H-1 NMR and ma...
GOKMEN, IG; ABDELQADER, E (Royal Society of Chemistry (RSC), 1994-04-01)
A simple and sensitive catalytic spectrophotometric method was developed for the determination of selenium in biological matrices. The method is based on the catalytic effect of selenium on the reaction of Methylene Blue (MB) with sodium sulfide. For a given reaction between MB and sodium sulfide, the change in the MB absorbance with time was monitored, then the time (t) required for completion of the reaction was determined, and t(-1) was calculated. A plot of t(-1) versus selenium concentration constitute...
Citation Formats
E. Boyacı, A. Rodriguez-Lafuente, B. Bojko, and J. Pawliszyn, “Introduction of solid-phase microextraction as a high-throughput sample preparation tool in laboratory analysis of prohibited substances,” ANALYTICA CHIMICA ACTA, pp. 69–81, 2014, Accessed: 00, 2020. [Online]. Available: