Simple Analytical Strategy for Screening Three Synthetic Cathinones (α-PVT, α-PVP, and MDPV) in Oral Fluids

Synthetic cathinones are analogue compounds of the plant based stimulant cathinone. Its use, abuse, and related consumption complications have steadily increased in the last years. For this reason, there is a need for innovative analytical approaches that enable its rapid screening in biological matrices (e.g., oral fluids). The present work proposes a new analytical methodology by combining bar adsorptive microextraction followed by microliquid desorption and gas chromatography coupled to mass spectrometry (BAµE-µLD/GC-MS) for screening three synthetic cathinones (α-PVP, α-PVT, and MDPV) in oral fluids. The optimization of the BAµE-µLD/GC-MS methodology was successfully applied for the analysis of the target compounds in oral fluids. The results show average recoveries between 43.1 and 52.3% for the three synthetic cathinones. Good selectivity was also noticed. The developed methodology presents itself as an alternative tool to screen these compounds in oral fluids. To the best of our knowledge, this is the first work that combines a microextraction sorption-based technique followed by GC-MS analysis for the screening of synthetic cathinones in oral fluids.

Spectroscopic Estimation of Doxylamine Succinate in Tablets and Human Plasma by Formation of Ion-pair Complex

Aim: To develop a simple spectroscopic method for estimation of doxylamine (DOX) succinate in its tablet dosage form and human plasma with the aid of an ion-pair complex formation. Methods: In this method, methyl orange (0.05 % w/v) dye was used to form an ion-pair complex in acetate buffer (1M; pH: 5.00) at 300 C ± 20C. The ion-pair complex formed was extracted with chloroform. The maximum absorbance for the ion-pair complex was measured at 420 nm. Results and discussion: The method conditions were obeyed Beer's law in the concentrations ranging from 5-25 µg/mL of DOX succinate with a correlation coefficient (r2) of 0.992. The ion-pair (drug-dye) complex was formed in a 1:1 ratio which was demonstrated by Jobs' method of continuous variation. The method was satisfied the validation criteria as per ICH (Q2R1) guidelines. Accuracy studies showed 99.06-100.9 % recovery of the analyte. The responses of the precision and robustness were found within acceptable limits (<2% RSD). The LOD and LOQ values were found as 0.31 and 0.939 µg/mL, respectively. Conclusion: The developed method was simple, specific, and economical and requires a short analysis time. Therefore it could be considered for precise analysis of DOX succinate in biological matrices.

Review on in vivo profiling of drug metabolites with LC-MS/MS in the past decade

Metabolite profiling is an indispensable part of drug discovery and development, enabling a comprehensive understanding of the drug's metabolic behavior. Liquid chromatography-mass spectrometry facilitates metabolite profiling by reducing sample complexity and providing high sensitivity. This review discusses the in vivo metabolite profiling involving LC-MS/MS and the utilization of QTOF, QQQ mass analyzers with a particular emphasis on a mass filter. Further, a summary of sample extraction procedures in biological matrices such as plasma, urine, feces, serum and hair as in vivo samples are outlined. toward the end, we present 15 case studies in biological matrices and their LC-MS/MS conditions to understand the metabolic disposition.