Analysis and Occurrence of 14 Sulfonamide Antibacterials and Chloramphenicol in Honey by Solid-Phase Extraction Followed by LC/MS/MS Analysis

Abstract

A method was developed for the analysis of 14 sulfonamide antibiotics and chloramphenicol in honey. These antibiotics have been banned for use in food-producing animals; yet, their residues were found in many samples, illustrating the need for a multiresidue analysis for these antibiotics in honey. The method described here uses an acid hydrolysis step to liberate the sugar-bound sulfonamides followed by a solid-phase extraction to remove potential interferences. Analysis was by liquid chromatography--electrospray ionization--tandem mass spectrometry in negative mode for all 15 analytes. This MRM method generated two structurally significant transitions per compound, and it was designed to conform to U.S. Food and Drug Administration MS confirmation guidelines. It also provides 4-EU identification points. One hundred sixteen samples from 25 countries were analyzed, and 38% were found to contain at least one target antimicrobial. Five different target compounds were found in honey from 13 different countries.

The challenges of developing a generic extraction procedure to analyze multi‐class veterinary drug residues in milk and honey using ultra‐high pressure liquid chromatography quadrupole time‐of‐flight mass spectrometry

“…Consequently, the method of Experiment IV was adopted and validated for the determination of the veterinary drugs that are listed in Table 1 in honey and milk. It should be noted that sulfonamides present in honey bind to the sugars, and the samples were typically subjected to acid hydrolysis, for example in 2 M HCl for 1 h at 50 C, [21] to liberate them and to detect the free form. In the current study, the acid hydrolysis was not applied and it was assumed that the QuEChERs method only extracted free sulfonamides present in honey samples.…”

Development of a rapid method for the determination of antibiotic residues in honey using UPLC-ESI-MS/MS

“…Dn the other hand, the isolation of sulfonamides from other honey components was performed by solid phase extraction (SPE) (Kaufmann et al, 2002;Maudens et al, 2004;Thompson & Noot, 2005). Moreover, analysis by liquid chromatography followed by fluorescence or ultra-violet detection systems can give low detection limits (Maudens et al, 2004;Pang et al, 2003;Posyniak et al, 2003;Sheridan et al, 2008) Recently, the basic advances in developing sensitivity and specifity of food analyses of pharmaceutical residues are due to the novel technology instrument, the application of ultra-performance liquid chromatography with tandem mass spectrometric detection (UPLC-MS/MS), which is more sophisticated technique allows a very effective isolation of analyte ions from the noise-producing matrix. The UPLC-MS/MS produces a high speed of analysis, greater resolution, higher peak capacity and sensitivity (Swartz 2005;Tamošiūnas & Padarauskas, 2008).…”

A rapid and sensitive LC-MS/MS method for the determination of multi-class residues of antibiotics in chicken liver

“…Sulfonamides (antibiotics) such as sulfaguanidine and sulfathiazole, which were included in this study, have been determined by HPLC-MS in honey with limits of detection (LODs) ranging between 10 and 50 µg kg -1 . [10][11][12] Using a C18 solid phase extraction cartridge for sample preparation and an ultra-triple quadrupole mass spectrometer, LODs as low as 0.06-0.18 µg kg -1 for sulfonamides in honey 13 have been reported in the literature. Another study employing a triple quadrupole mass spectrometer 14 demonstrated that the matrix influences the determination of sulfonamides.…”