QuEChERS-超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速测定水产品中25种药物残留

采用了一种高效基质脂肪吸附剂（EMR-Lipid）去除水产品基质中的脂肪和磷脂等杂质，利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法（UPLC-Q Orbitrap HRMS）的同时定性定量功能，建立了水产品中25种药物残留的检测方法。样品经乙腈提取，EMR-Lipid净化，同时加入3 g氯化钠和3 g无水硫酸钠进行盐析，采用ACQUITY UPLC BEH C18色谱柱（100 mm×2.1 mm，1.7 μm）分离，以含0.1%（v/v）甲酸的乙腈溶液和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，在加热电喷雾离子（HESI）源、全扫描/实时二级质谱扫描（Full MS/dd-MS²）监测模式下进行检测。结果表明，25种目标化合物的质量浓度与母离子峰面积间的线性关系良好，相关系数（r）均大于0.997；25种目标化合物的检出限为0.1~1.0 μg/kg，其平均加标回收率为70.1%~108.9%，相对标准偏差为2.1%~13.8%。该法具有操作简单快捷、灵敏度高等优点。

Rapid determination of 25 drug residues in aquatic products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q Orbitrap HRMS) method was developed for the rapid screening of 25 drug residues in aquatic products by the application of a novel enhanced matrix removal of lipids (EMR-Lipid). The samples were extracted with acetonitrile, cleaned-up with EMR-Lipid, and salted out with 3.0 g sodium chloride and 3.0 g sodium sulfate. The separation of the 25 drug residues was performed on an ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) with gradient elution. Acetonitrile containing 0.1% (v/v) formic acid and 0.1% (v/v) formic acid aqueous solution were used as mobile phases. The compounds were detected by Full scan/date dependent MS/MS (Full MS/dd-MS²) via heated electrospray ionization (HESI) source. The calibration curves were linear with correlation coefficients (r) greater than 0.997. The limits of detection (LODs) ranged from 0.1 μg/kg to 1.0 μg/kg. The average spiked recoveries of the 25 target compounds were between 70.1% and 108.9% with relative standard derivations (RSDs) from 2.1% to 13.8%. Compared with the previous methods, this method has characteristics of simpler sample preparation and higher sensitivity.