Rapid Screening And Quantification Of Multi-Class Multi-Residue Veterinary Drugs In Pork By A Modified Quechers Protocol Coupled To UPLC-QOrbitrap HRMS
A rapid and simple analytical method for the screening and quantification of multi-residues was established by a quick, easy, cheap, effective, rugged and safe (QuEChERS) approach coupled to ultra-performance liquid chromatography and electrospray ionization quadrupole orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). A total number of 59 veterinary drugs were investigated, which belonged to 12 classes, such as β-agonist, quinolones, sulfonamides, tetracyclines, lincomycin series, triphenylmethane, nitroimidazoles, macrolides, amide alcohols, quinoxalines, steroid hormone and sedatives.
The factors which influence the determination of veterinary drugs residues, such as mobile phase, extract solvent, clean up sorbent, and re-dissolved solvent, were optimized by the single factor experiment. The method was sufficiently validated by using the parameters of linearity, sensitivity, accuracy, and repeatability.
The response of the detector was linear for 59 veterinary drug residues in extensive range (two to three orders of magnitude) with a high coefficient of determination (R2) (0.9995-0.9998). The limit of quantification (LOQ) ranged from 0.1μg/kg to 2.0μg/kg for 59 veterinary drug residues in pork samples. The repeatability was in the range of 1.0%-9.5%. Average recoveries of 59 veterinary drugs at three spiked levels ranged from 53.7%-117.8% with relative standard deviation (RSD) of 1.9%-13.9%. The full MS scan coupled with data-dependent MS/MS mode was applied for screening the target compounds to simultaneously obtain the accurate mass of parent ion and the mass spectrum of fragments. Elemental composition, accurate mass, and retention time and characteristic fragment ions were used to establish a homemade database.
The ability of the homemade database was verified by analyzing the real pork samples, and the result was satisfactory.