Novel capsule phase microextraction - Gas chromatography - Mass spectrometry for analysis of pheniramine in a case of its fatal intoxication

Abstract

In forensic toxicology, the extraction and purification of analytes from complex biological matrices heavily rely on the effectiveness of sample preparation methods. However, existing methods often face inherent challenges such as interfering substances and limited sample quantities, which can compromise the accuracy and efficiency of toxicological analyses. In the present work, for the first time, capsule phase microextraction (CPME) was implemented in forensic toxicology casework for the straightforward, affordable and sustainable extraction of the pheniramine (PHN) drug from human autopsy samples (whole blood and liver) and determined by GC-MS. A systematic investigation was conducted to optimize the extraction efficiency of CPME by examining and optimizing significant variables such as pH and volume of sample, adsorption time, desorption time and volume. The optimized method demonstrated linearity, covering a range of 0.1–10 μg mL−1 for blood samples and 0.1–10 μg g−1 for liver samples. The limit of quantification (LOQ) of the method for PHN in blood and liver samples was determined to be 0.063 μg mL−1 and 0.076 μg g−1, respectively. Repeatability and reproducibility of the method were less than 3.2% and 9.2%, respectively. The method demonstrated accuracy and recovery within the ranges of 94%–101.3%, and 67.4%–82%, respectively. The method was applied for analysis of autopsy samples from a case of fatal PHN intoxication and results were compared to those obtained using the conventional solid-phase extraction (SPE) method. Further, the competence of the proposed method has been judged by White Analytical Chemistry (WAC) RGB12 algorithm. CPME-GC-MS method demonstrates notable performance and significant stride in the domain of postmortem toxicology sample preparation. It is superior to traditional methods in several ways such as simpler, more sustainable, affordable and overcome the challenges of interfering substances and limited sample quantity.