Application of microextraction by packed sorbent to isolation of psychotropic drugs from human serum

A method of microextraction by packed sorbent (MEPS) followed by liquid chromatography with diode array detection has been developed and optimized for the extraction of six tricyclic antidepressants (amitriptyline, nortriptyline, imipramine, desipramine, doxepin, nordoxepin) from human serum. The optimal parameters of MEPS extraction (type of sorbent, volume of sample, composition, and volume of washing and elution solutions) for these drugs in spiked samples were defined. The developed MEPS procedure was validated and then successfully applied to the analysis of serum reference material. The limit of detection (0.02–0.05 μg/mL), intraday (2.7–8.8%) and interday (4.4–11.6%) precision (RSD), and the accuracy of the assay (94.5–108.8%) at three concentration levels—0.2, 0.5, and 0.8 μg/mL—were estimated. The accuracy of the method was evaluated by the analysis of certified reference material. Moreover, the validated procedure was compared with the solid-phase extraction technique. Finally, microextraction by packed sorbent was assessed as a suitable tool in forensic and clinical methods for serum sample preparations

The 42nd Symposium Chromatographic Methods of Investigating Organic Compounds : Book of abstracts

The 42nd Symposium Chromatographic Methods of Investigating Organic Compounds : Book of abstracts. June 4-7, 2019, Szczyrk, Polan

Development of microextraction by packed sorbent for toxicological analysis of tricyclic antidepressant drugs in human oral fluid

The aim of this study was to apply microextraction by packed sorbent (MEPS) to the isolation of six tricyclic antidepressants (TCADs): nordoxepin, doxepin, desipramine, nortriptyline, imipramine, and amitripty- line from human oral fluid. Samples were collected from healthy volunteers via free spillage from the oral cavity to disposable test tubes. A method of oral fluid sample pretreatment was developed and optimized in terms of suitability for MEPS extraction and removing of interfering agents (protein, food debris, or air bubbles). Moreover, it was short and simple to perform with limited sample consumption (150 L). Extracts were analysed by UHPLC–MS. The MEPS/UHPLC–MS method was validated at three concentration levels (2.00, 4.00 and 8.00 ng/mL) of all analytes in the range 1.25–10.0 ng/mL. The follow- ing parameters were determined: limit of detection, limit of quantification, precision, and accuracy. For all tested concentration levels, the intra- and inter-day repeatability did not exceeded 8.1% and 12.2%, respectively. Gained LOQ value, 0.50 ng/mL, made the MEPS/UHPLC–MS method to be a useful tool in clinical and forensic laboratories, which was demonstrated on the basis of analysis of real samples

Electrochemical sensor for determination of desipramine in biological material

AbstractA simple electrochemical method for determination of desipramine in human oral fluid was developed. Two types of electrodes, namely: glassy carbon electrode (GCE) and screen-printed electrode (SPE) were tested with different electrochemical techniques: cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The simplex method was applied to find optimal instrumental conditions of DPV measurements. Three parameters were subjected to optimization with the simplex method procedure, namely potential of the pulse (Ep), potential difference between pulses (Es) and pulse time (tp). Buffer solution pH and material of the working electrode were tested in a pre-optimization step. For optimal working conditions of a given screen-printed electrode two ranges of desipramine concentration were tested. Signals registered for desipramine within the range of 0.01-1μM enabled its determination in alternative biological material such as saliva