QuEChERS/UPLC-Q-OrbitrapHRMS法测定水产及水产加工品中16种苯并咪唑类与13种硝基咪唑类药物残留

Determination of 16 Benzimidazoles and 13 Nitroimidazoles Residues in Fish and Fishery Products by UPLC-Q-OrbitrapHRMS with QuEChERS

建立了Qu ECh ERS/超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-OrbitrapHRMS)同时检测水产及水产加工品中16种苯并咪唑类和13种硝基咪唑类药物残留的分析方法。样品经乙酸乙酯提取,浓缩近干,用30%(体积分数)甲醇-水溶液定容,乙腈饱和正己烷、氨基(NH2)吸附剂和Mg SO4净化。采用Thermo fisher Accucore RP-MS色谱柱(100 mm×2.1 mm,2.6μm),以0.1%(体积分数)甲酸-乙腈为流动相进行梯度洗脱,使用可加热电喷雾离子源(HESI),全扫描/数据依赖二级扫描(Full MS/dd-MS2,Top N=1)模式检测,外标法定量。结果表明,29种药物在0.5~400μg/L范围内线性关系良好(r2≥0.9967),在5种水产及水产加工品基质中进行3个不同水平的加标实验,平均回收率为60.2%~123.3%,相对标准偏差(n=6)为0.1%~21.7%,方法的定量下限为0.5~5.0μg/kg。该法操作简便、精密度高、准确性好,适用于批量水产及水产加工品中29种药物的快速检测。

A method was developed for the simultaneous determination of 16 benzimidazoles and 13 nitroimidazoles residues in fish and fishery products using ultrahigh performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry（UPLC-Q-OrbitrapHRMS）. The samples were extracted with ethyl acetate,then concentrated and dissolved with 30%methanol aqueous solution,and cleaned up using hexane saturated with acetonitrile,amine（NH2）sorbent and Mg SO4. The separation was performed on a Thermo fisher Accucore RP-MS（100 mm ×2. 1 mm,2. 6 μm） column using acetonitrile and 0. 1% formic acid as mobile phase by gradient elution. The analytes were analyzed in Full MS/dd-MS2（Top N = 1） mode with a heated electrospray ion source（HESI）,and quantified by the external standard method. The calibration curves for the29 analytes were linear in the range of 0. 5-400 μg/L with correlation coefficients not less than0. 996 7. The average recoveries at three spiked levels in 5 kinds of product matrixes ranged from60. 2% to 123. 3% with relative standard deviations（RSDs,n = 6） of 0. 1%-21. 7%. The limits of quantitation were 0. 5-5. 0 μg/kg. With the advantages of simplicity,high precision and good accuracy,the method is suitable for the rapid detection of 29 veterinary drug residues in aquatic products.