Determination of Acetaminophen, Dexchlorpheniramine, Caffeine, Cotinine and Salicylic acid in 100 μL of Whole Blood by UHPLC–MS/MS

Abstract

A sensitive and robust ultra-high-performance liquid chromatography-tandem mass spectrometry method has been developed and validated for the quantification of acetaminophen, dexchlorpheniramine, caffeine, cotinine and salicylic acid in postmortem blood samples from children younger than 4 years. The sample was prepared by a protein precipitation with ice-cold methanol/acetonitrile mixture (85:15, v/v). The organic phase was evaporated to dryness and the residue was dissolved in the mobile phase. Separation, with gradient elution and an acidic mobile phase, was achieved on an Acquity UPLC® HSS T3 column. The compounds were quantified using a multiple reaction-monitoring mode. Two transitions were monitored for each compound and one for the deuterated internal standards. The mass spectrometric detection in the positive ion mode was performed for all the compounds except salicylic acid which was detected in the negative ionization mode. The limits of quantification were as follows: acetaminophen 0.30 mg/L, dexchlorpheniramine 0.0050 mg/L, caffeine 0.099 mg/L, cotinine 0.00035 mg/L and salicylic acid 1.3 mg/L. Between-assay and within-assay precisions were ≤15% (biases: -10% to 26%) and ≤10%, respectively. Extraction recoveries varied from 93% to 137%. The matrix effects in blood, corrected with deuterated internal standards, were 100% ± 10% for all compounds except dexchlorpheniramine (111%) and caffeine (138%).

Adsorptive stripping voltammetric method for the determination of caffeine at integrated three-electrode screen-printed sensor with carbon/carbon nanofibers working electrode

“…Many different procedures have been proposed for assay a caffeine in biological and pharmaceutical samples including gas chromatography/mass spectrometry (GC/MS) (Jeon et al 2017), liquid chromatography/mass spectrometry (LC-MS) (Li et al 2015), liquid chromatography using fluorimetric and UV detection (Ibrahim and Wahba 2014), high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) (Rybak et al 2014), ultra-high-performance liquid chromatography-tandem mass spectrometry method (UHPLC-MS/MS) (Krpo et al 2018;Liu et al 2013) and also solid surface fluorescence using membrane filters modified with MWCNTs (Talio et al 2013) or multivariate calibration-prediction techniques, principal component regression (PCR), partial least squares (PLS) and artificial neural networks (ANN) were applied to the spectrometric multicomponent analysis (Aktaş and Kitiş 2014). However, these methods are generally expensive and often require a tedious, time-consuming sample pretreatment, which makes them unsuitable for the routine analysis of large number of samples.…”

Poly[(2‐(acryloyloxy) ethyl]trimethylammonium chloride‐co‐ethylene dimethacrylate monolith on‐line solid‐phase extraction coupled with liquid chromatography and tandem mass spectrometry for the fast determination of salicylic acid in foodstuffs

“…SA (and its salicylate anion) is the principal metabolite of ASA and it is the pharmacologically active substance in food and biological samples [6]. Many chromatographic methods including CE [7], LC-UV [8,9], and LC-MS/MS [10][11][12][13] have been proposed for the analysis of SA in food and biological samples. The residues present in food samples are usually at extremely low concentrations with complex and multicomponent matrixes.…”

γ-Fe2O3/CNTs Composites for Electrochemical Detection of Paracetamol: Synthesis, Phase Transition and Enhanced Properties

“…However, it is still difficult to detect a substance with very low concentration. At present, titration method, 8,9 chemical spectroscopy, 10 HPLC, 11,12 ultra-highperformance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), 13 and spectrophotometry 14,15 are often used for the determination of paracetamol. However, these methods usually require tedious sample pretreatment and are not conducive to the analysis anytime and anywhere.…”