Green Analytical Chemistry (Mar 2025)
Optimization of VA-DLLME methodology for the determination of beta-cyfluthrin in blood and urine sample of human by TLC-image analysis: Validated by AGREE and complex GAPI tools
Abstract
Beta-cyfluthrin is an insecticide that belongs to the category of pyrethroid pesticide which is considered a “highly hazardous” substance and is often misused in different countries, leading to self-poisoning. Forensic toxicology laboratories frequently encounter pesticide poisoning due to its severe effects. The current research presents an affordable analytical method that combines Vortex-Assisted Dispersive Liquid-Liquid Microextraction to Thin Layer Chromatography Imaging System(DLLME-TLC-IS) that, is fast, efficient, safe, and green(er) to the environment. In this research, 20 µL of the extract obtained by DLLME-TLC-IS was applied to a thin layer chromatography (TLC) plate by using a developing solvent ethyl acetate: hexane (1:1). The TLC plate was then analysed using the free software ImageJ after being exposed to ultraviolet light at 254 nm. Various extraction parameters were tested, including pH, ionic strength, type and volume of extraction and disperser solvent., and vortex speed and time. After optimizing these conditions, the limit of detection (LOD) was observed to be 0.45 µg/spot in blood samples and 0.94 µg/spot in urine samples. At the same time, the limit of quantification (LOQ) was 0.29 µg/spot in blood and 0.9 µg/spot in urine samples respectively. The method demonstrated linearity in the range of 1–10 µg/spot, with a correlation coefficient of determination of 0.9912 for blood and 0.9931 for urine. Beta-cyfluthrin recoveries were 96 % in blood and 99 % in urine samples, respectively. Overall, this developed method for detecting beta-cyfluthrin in human blood and urine samples is efficient, cost-effective, and adheres to the principles of green analytical chemistry(GAC). This approach offers advantages over previously established methods. The green characteristics of the developed method were assessed using complexGAPI and AGREE tools of greenness.
