Assessment of the impact of hydrolysis on bound sulfonamide residue determination in honey using stable isotope dilution ultrahigh performance liquid chromatography tandem mass spectrometry

In this study, an analytical method based on isotope dilution-liquid chromatography tandem mass spectrometry (ID-LC-MS/MS) was developed as a candidate reference method for the determination of sulfonamides (SAs) in honey. To guarantee the accuracy and authenticity, the impact of hydrolysis on bound SA residues was first investigated by enabling (i) identification of sugar-bound SAs, (ii) clarifying the binding reaction rule between the SAs and sugar, (iii) detection of free SAs and sugar-bound SAs, and (iv) preparation of SA-contaminated honey. Thus, the efficiency of different hydrolysis conditions was assessed by comparing the bound SA content before and after hydrolysis. In addition, optimization of the sample pretreatment procedures and LC conditions to minimize matrix effects by separation from significant matrix interferences was also performed. Satisfactory results in terms of hydrolysis efficiency (approximately 88.3%-99.2%), extraction efficiency (84.2%-105.3%), recovery (95.9%-103.1%), and limit of quantification (0.6-1.5 mu g.kg(-1)) were obtained.

Automated summary

An analytical method based on ID-LC-MS/MS was developed for determining sulfonamides in honey. The impact of hydrolysis on bound SA residues was investigated, along with optimization of sample pretreatment procedures to minimize matrix effects, resulting in efficient hydrolysis, extraction, recovery, and low limit of quantification.