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.%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.
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