BACKGROUND:
A rapid and simple analytical method for the screening and quantification of multi residues was established by 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.
METHODS:
The factors which influence the determination of veterinary drugs residues, such as mobile phase, extract solvent, clean up sorbent, re-dissolved solvent, was optimized by single factor experiment. The method was sufficiently validated by using the parameters of linearity, sensitivity, accuracy, and repeatability.
RESULTS:
The response of detector was linear for 59 veterinary drug residues in extensive range (two to three orders of magnitude) with high coefficient of determination (R2) (0.9995-0.9998). The limit of quantification (LOQ) was from 0.1μg/kg to 2.0μg/kg for 59 veterinary drug residues in pork samples. The repeatability was at the range of 1.0%-9.5%. Average recoveries of 59 veterinary drugs at three spiked levels ranged of 53.7%-117.8% with relative standard deviation (RSD) of 1.9%-13.9%. The full MS scans 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.
CONCLUSION:
The ability of the homemade database was verified by analyzing the real pork samples, and the result was satisfactory.