Background: 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.

Methods: 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.

Results: 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.

Conclusion: The ability of the homemade database was verified by analyzing the real pork samples, and the result was satisfactory.

背景：快速，简便，廉价，有效，坚固耐用且安全的（QuEChERS）方法与超高效液相色谱和电喷雾电离四极杆Orbitrap高效液相色谱法相结合，建立了一种快速，简单的分析方法，用于多残留物的筛选和定量。分辨率质谱（UPLC-Q-Orbitrap HRMS）。共调查了59种兽药，它们属于12类，如β-激动剂，喹诺酮类，磺酰胺类，四环素类，林可霉素系列，三苯甲烷，硝基咪唑类，大环内酯类，酰胺醇类，喹喔啉类，类固醇激素和镇静剂。

方法：通过单因素实验，优化影响兽药残留测定的因素，如流动相，萃取溶剂，净化吸附剂和再溶解溶剂。通过使用线性，灵敏度，准确性和可重复性参数充分验证了该方法。

结果：检测器对宽范围（2-3个数量级）中的59种兽药残留具有线性，并具有较高的测定系数（R2）（0.9995-0.9998）。猪肉样品中59种兽药残留的定量限（LOQ）为0.1μg/ kg至2.0μg/ kg。重复性在1.0％-9.5％的范围内。三个加标水平的59种兽药的平均回收率在53.7％-117.8％之间，相对标准偏差（RSD）为1.9％-13.9％。完整的MS扫描结合数据依赖的MS / MS模式用于筛选目标化合物，以同时获得准确的母体离子质量和碎片质谱。使用元素组成，准确的质量，保留时间和特征性碎片离子来建立自制数据库。

结论：通过对真实猪肉样品的分析验证了自制数据库的能力，结果令人满意。