Liquid Chromatography–Mass Spectrometry/Mass Spectrometry Method Development for the Determination of Carbaryl Residue in Honey

Objective: Liquid chromatography– mass spectrometry/mass spectrometry (LC‑MS/MS) method development for the determination of Carbaryl insecticide in honey and Comparisons of different extraction techniques to determine the efficiency of extraction process. Materials and Methods: The LC‑MS/MS method was developed by optimizing the multiple reaction monitoring (MRM) parameters. Further, the comparison study was done for the optimized extraction techniques such as quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and ultrasound solid phase extraction (SPE) in the developed method. The validation was studied for the developed method as well as the extraction techniques to confirm the robustness of the developed method. Results: The validation study showed good accuracy for the developed method for the concentration from 2 to 9 ppb of the working solution. Limit of detection for the developed method was 0.08 and 0.05 ppb for the fragments 145.1 m/z and 127.1 m/z, respectively. Moreover, limit of quantification for the fragment 145.1 m/z was 0.24 ppb and for 127.1 m/z was 0.16 ppb. The average accuracies for the developed method of both the fragments (145.1 m/z and 127.1 m/z) were 98.51% and 98.15%, respectively. Recovery percentage for optimized QuEChERS ranged from 107% to 112% and for the ultrasound‑SPE and from 107% to 118% of the honey samples which were spiked with three different concentrations of analyte. Conclusion: From the validation, it was confirmed that the developed method was robust and simple and provides better sensitivity and intensity and low consumption of chemicals. Thus, the developed method can be used for the routine analysis of carbaryl in honey.