超高效液相色谱-四级杆-飞行时间质谱法同时快速检测水产品中37种兽药残留

Determination of 37 kinds of veterinary drugs residues in aquatic products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

中文关键词:  水产品  兽药残留  筛查  同时检测  超高效液相色谱-四级杆-飞行时间质谱法

英文关键词:aquatic products  veterinary drugs residues  screening  simultaneous determination  ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-四极杆-飞行时间质谱法快速检测水产品中磺胺类、喹诺酮类、四环素类、硝基咪唑类、大环内酯类、β-内酰胺类、三苯甲烷类7类37种兽药残留的方法。方法 样品采用QuEChERS方法(quick, easy, cheap, effective, rugged and safe method)进行前处理(用乙腈提取, 提取液经Al2O3吸附剂净化); 采用ZORBAX SB-C18 色谱柱(100 mm×2.1 mm, 3.5 μm)分离, 以乙腈- 5 mmol的乙酸铵为流动相, 梯度洗脱, Q-TOF-MS电喷雾正离子模式分析检测; 在全扫描采集模式下, 以准分子离子峰的峰面积定量, 以化合物的色谱保留时间和精确质量数定性。结果 各化合物在0.5~2000 μg/kg范围内均呈现良好的线性关系, 相关系数均大于0.99。样品平均添加回收率为 67%~109.5%, 相对标准偏差(RSD)均小于15.3% (n=6)。结论 方法简单、快速、可靠, 可用于水产品中兽药多残留的快速筛查。

英文摘要:

      Objective To establish a method for the simultaneous determination of 7 classes of 37 kinds of veterinary drugs, including sulfoamides, quinolones, tetracyclines, nitroimidazoles, macrolides, beta-lactams and triphenylmethane, in aquatic products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS). Methods The quick, easy, cheap, effective, rugged and safe method (QuEChERS) was used for the extraction. In this QuEChERS method, the sample was extracted by acetonitrile and cleaned up with Al2O3. The compounds were measured on a ZORBAX SB-C18 column (100 mm×2.1 mm, 3.5 μm) with acetonitrile- 5 mmol/L ammonium acetate as mobile phase under gradient elution. The extract was measured directly by LC-Q TOF-MS with electrospray ionization in positive mode. The confirmatory analysis was carried out by determining the retention time and accurate masses of all compounds and fragment ions upon target MS/MS. Results The results showed that the linear range was 0.5~2000 μg/kg for each compound with the correlation coefficients of more than 0.99. The recoveries were ranged from 67.0% to 109.5% , with relative standard deviations (RSDs) less than 15.3% (n=6). Conclusion The method is simple, rapid and reliable, and is suitable for the simultaneous determination of multiresidues of veterinary drugs in aquatic products.