A green deep eutectic solvent based dispersive liquid-liquid microextraction for the quantitative analysis of 21 polychlorinated biphenyl metabolites in food of animal origin using injector port silylation-gas chromatography-tandem mass spectrometry.

An analytical method was developed for the quantitative determination of 21 polychlorinated biphenyls (PCBs) metabolites (17 were -OH, 1 -MeO, and 3 were MeSO2) in foods of animal origin using deep eutectic solvent (DES) based dispersive liquid-liquid microextraction followed by injector port silylation-gas chromatography-tandem mass spectrometry. The type of DES (thymol: camphor, 1:1 molar ratio) and optimum volume of DES (300 µL), pH (7.0), and disperser solvent (acetonitrile) were optimized to attain the maximum extraction efficiency. The limit of detection, limit of quantification, and percent recovery were found to be in the range of 0.12-0.23 ng/mL, 0.40-0.76 ng/mL, and 80.1-111.4%, respectively. The expanded uncertainty was observed to be in the range of 7.2-22.8% for the targeted analytes. The proposed method was applied to real food samples (milk, meat, fish, and egg) and the levels were found to be in the range of 0.64-32.14 ng/g. This is first of its kind method using green solvent based method for the analysis of PCB metabolites (-OH, MeO, and MeSO2) and will find extensive application in routine testing for foods of animal origin.

Experimental design of non-ionic hydrophobic DES-DLLME coupled with injector port silylation-GC-MS/MS for the quantitative determination of 13 bisphenols in food samples.

Non-ionic hydrophobic deep eutectic solvent based DLLME method with thymol and camphor (1:1 mole ratio) as extraction solvent and acetonitrile as disperser solvent was developed for the determination of 13 bisphenols (BPs) in food commodities by auto IPS-GC-MS/MS. Further, the influential parameters pH, vortex time, and volume of NIHDES for extraction of 13 BPs were optimized by employing the design of experiment. The LOQ and recoveries were observed to be 0.1 ng mL-1, and 77.8-109.2%, respectively. The expanded uncertainty was found to be 4.8-18.0% for the developed and validated method, which was applied to food commodities to determine 13 BPs and their levels were in the range of 0.01-1.24 ng mL-1 in liquid foods (milk, water, and beverages) and 0.29-3.25 ng g-1 in meat samples (goat, chicken, and fish). The present green analytical method is highly suitable for the rapid determination of 13 BPs in food commodities for routine analysis.