Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of sulfonamides, trimethoprim and dapsone in muscle, egg, milk and honey

Abstract

A quantitative multi-residue method that includes 13 sulfonamides, trimethoprim and dapsone was developed and validated according to Commission Decision 2002/657/EC for muscle, milk egg and honey samples. For all matrices, the same extraction procedure was used. Samples were extracted with an acetone/dichloromethane mixture and cleaned up on aromatic sulfonic acid (SO3H) SPE cartridges. After elution and concentration steps, analytes were identified and quantified by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Data were acquired according to the multiple reaction-monitoring approach (MRM) and analytes were quantified both by the isotope dilution and the matrix-matched approaches calculating the response factors for the scanned product ions. The developed method shows good linearity, specificity, precision (repeatability and within-laboratory reproducibility), and trueness. Estimated CCβ for sulfonamides ranged between 5.6 and 8.2 µg kg(-1) for eggs, between 11.1 and 69.9 µg kg(-1) for milk, between 64.7 and 87.9 µg kg(-1) for muscle, and between 2.7 and 5.3 µg kg(-1) for honey. CCβ values for dapsone were 3.1, 0.6, 0.7 and 1.5 µg kg(-1) and for trimethoprim were 3.1, 6.7, 81.7 and 3.0 µg kg(-1) calculated for eggs, milk, muscle and honey, respectively. Recovery for all matrices was in the range from 89.1% and 109.7%. In matrix effect testing, no significant deviations were found between different samples of muscle and milk; however, a matrix effect was observed when testing different types of honey. The validation results demonstrate that the method is suitable for routine veterinary drug analysis and confirmation of suspect samples.

Trends in sensitive detection and rapid removal of sulfonamides: A review

“…As a confirmatory detector, MS can provide information about the molecular structures and quantitative data on the analytes with high sensitivity and selectivity. Furthermore, for the purpose of enhancing sensitivity and accuracy, MS/MS [50,51,53,55] has been utilized for the analyses of sulfonamides. With the advantages and disadvantages mentioned above, MS/MS is outstanding compared with the other detectors.…”

Residue Determination in Honey

“…Moreover, after derivatization with fluorescamine, sulphonamides give fluorescence and some procedures apply LC-FLD (with pre-or post-column derivatization), reaching limits of detections (LOD/CCβ) comparable to those of LC-MS methods. In Table 9, some example of these applications are listed [69][70][71][72][73][74][75][76][77][78]. Since considerable amounts of SAs are bound to honey sugars, in 2000 Schwaiger and Schuch [79] demonstrated the need of an acidic hydrolysis prior to the residue analysis.…”

“…Therefore, at one hand, exploiting their basic moiety, some procedures use strong cation exchange (SCX-SPE) to isolate sulphonamides from the acidic honey extracts [71][72][73]77]. On the other hand, to successfully apply RP-SPE or LLE clean-up, some researchers buffered honey extract in the pH range about 4-6 in which the neutral form of sulphonamides prevails [70,[74][75][76]78]. In this interval, the distribution coefficients (D) reach their maximum and the compound lipophilicity is enhanced, as shown in Figure 3 for sulphathiazole.…”

Rapid determination of sulfonamide residues in honey samples using non‐targeted liquid chromatography‐high resolution mass spectrometry

“…As a result, antibiotics can be detected at trace levels in honey [3]. Antibiotic residues (e.g., Sulfonamides) were found in various samples such as honey, milk, eggs, fish, or meat [4][5][6][7]. Recently, various strategies have been developed for the efficient analysis of SA residue in honey [8,9].…”