In the present work, we describe a simple, rapid, cost‐effective, environmentally friendly and high‐sample‐throughput analytical method based on coupling vortex‐assisted dispersive liquid–liquid microextraction with thin layer chromatography analysis for quantitative determination of acetaminophen in whole human blood and tissues of stomach and liver. Followed by dispersive liquid–liquid microextraction, 20 μL of sedimented phase (chloroform) was spotted on a thin layer chromatography plate and developed with mobile phase of chloroform: acetone (8:2, v/v). The developed plate was photographed under ultraviolet chamber at 254 nm and the image was processed for quantification of spots using freely available ImageJ software. Under the optimized conditions, the limit of detection and limit of quantification were found to be in the range of 7.74–8.33 and 23.4–25.2 μg/spot, respectively. The method was found to be linear in the range of 30–300 μg/spot with a coefficient of determination of 0.996 and 0.998 in blood and tissue, respectively. The developed method has been successfully applied for the determination of acetaminophen in autopsy samples from a case of acetaminophen overdose. The method does not require any sophisticated high‐end instrumentation and can be routinely applied for determination of acetaminophen in complex biological samples in resource‐limited laboratories.
A simple, rapid, cost‐effective and environment friendly analytical method based on dispersive liquid‐liquid microextraction (DLLME) coupled to injection port silylation (IPS)–gas chromatography‐mass spectrometry is described for the determination of morphine in illicit opium samples. Raw opium was dispersed in ultrapure water and 5 mL of aqueous sample was subjected to DLLME by rapidly injecting a mixture of chloroform and acetone (extraction and disperser solvent, respectively) followed by ultrasonication for 1 min and subsequent centrifugation for 3 min at 5000 rpm. The sedimented phase thus obtained was reconstituted in acetonitrile and 1 µL along with 1 µL of N,O‐Bis(trimethylsilyl)acetamide (BSA) was injected manually into GC‐MS injection port at a temperature of 250°C. The derivatization reaction was completed instantaneously inside the heated GC‐MS injection port without any side product. Various parameters associated with IPS and DLLME have been thoroughly optimized. Under the optimized conditions, the method has been found linear in the range of 5‐50 µg/mL with a correlation coefficient (R2) of 0.997. The limit of detection (LOD) and limit of quantification (LOQ) for morphine‐diTMS were found to be 1.6 and 4.8 µg/mL. The method has been successfully applied for the quantitative analysis of morphine in illicit opium samples. In conclusion, the proposed method has completely eliminated the time consuming and laborious steps of LLE and in‐vial silylation and can be routinely used for analysis of opium and other polar analytes in forensic science laboratories.
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