enhancing pesticide residue quantification in honey through integrated chemo-physical and chemometric separation using lc-ms spectrometry: comparison with multiple reaction monitoring

Honey, a naturally occurring product generated by bees, holds considerable nutritional and ethnomedicalsignificance. its constitution, primarily comprising carbohydrates and water, demonstrates variability rooted inthe sources of nectar. the widespread consumption of honey on a global scale has precipitated the imperativefor rigorous quality control and vigilance against contamination within commercial transactions. the utilizationof pesticides in agricultural practices, pivotal for augmenting yields, can engender the presence of pesticideresidues in foodstuffs, thereby necessitating the establishment of maximum residue limits (mrls). the mainobjective of the present study is to monitor residues of some major pesticides in honey samples collected fromimportant areas of honey production in the country. divergences in mrls across different nations haveengendered contentious discussions in international trade circles. the comprehensive analysis of pesticideresidues within honey demands the application of sophisticated methodologies owing to its intricate matrix [1].modern analytical techniques such as gc-ms/ms and uhplc-ms/ms, coupled with proficient extraction andpurification protocols, offer stringent detection thresholds for the analysis of multiple pesticide residues,congruent with established mrls. among these methods, lc-ms/ms in multiple reaction monitoring (mrm)mode emerges as a benchmark approach for the analysis of intricate samples [2]. this mode enables the selectiveisolation of target analytes while excluding background noise, delivering enhanced sensitivity andreproducibility. alternatively, lc-ms operated in full scan mode, reliant solely on a single-quadrupole massspectrometer, has the potential to circumvent challenges like peak overlapping. nevertheless, full scan lc-msis marked by a lack of selectivity, thereby complicating the resolution and precise quantification of targetedcompounds, particularly when compared to mrm. the phenomenon of overlapping peaks and the presence ofinterfering substances are commonplace in the quantitative analysis of complex samples like biological fluids.to surmount these intricacies, a shrewd approach capitalizing on three-way lc-ms data and second-ordercalibration was devised. this strategy achieves quantitative precision comparable to mrm, leveraging theconcept of mathematical separation in lieu of the conventional optimization of physical separations. thisinnovative strategy bestows amplified selectivity and sensitivity upon the analytical process. its practicality isunderscored by its efficiency, cost-effectiveness, and eco-friendliness, thus emerging as a viable alternative forthe precise determination of target analytes within intricate systems. in a specific project context, the analysisof 38 pesticides within honey samples was accomplished through the utilization of lc-ms data and advancedchemometric techniques. the inadequacies of the chromatographic approach in addressing peak separationintricacies were compensated through the employment of chemometrical separation. the integration offchemometrical and physico-chemical separation techniques led to a discernible augmentation in the selectivityof the analytical methodology.