QuEChERS/UPLC-Q-Orbitrap HRMS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 |
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基金项目:广东省省级科技计划项目(2015A050502010,2014A040401011) |
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中文摘要:建立了QuEChERS/超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)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MgSO4净化。采用Thermo fisher Accucore RP-MS色谱柱(100 mm×21 mm,26 μm),以01%(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,TopN=1)模式检测,外标法定量。结果表明,29种药物在05~400 μg/L范围内线性关系良好(r2≥0996 7),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602%~1233%,相对标准偏差(n=6)为01%~217%,方法的定量下限为05~50 μg/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。 |
中文关键词:四极杆/静电场轨道阱高分辨质谱(Q-Orbitrap HRMS) QuEChERS 水产及水产加工品 硝基咪唑类 苯并咪唑类 |
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Determination of 16 Benzimidazoles and 13 Nitroimidazoles Residues in Fish and Fishery Products by UPLC-Q-Orbitrap HRMS with QuEChERS |
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Abstract: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-Orbitrap HRMS).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 MgSO4.The separation was performed on a Thermo fisher Accucore RP-MS(100 mm×21 mm,26 μm) column using acetonitrile and 01%formic acid as mobile phase by gradient elution.The analytes were analyzed in Full MS/dd-MS2(TopN=1) mode with a heated electrospray ion source(HESI),and quantified by the external standard method.The calibration curves for the 29 analytes were linear in the range of 05-400 μg/L with correlation coefficients not less than 0996 7.The average recoveries at three spiked levels in 5 kinds of product matrixes ranged from 602%to 1233%with relative standard deviations(RSDs,n=6)of 01%-217%.The limits of quantitation were 05-50 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. |
Key Words:quadrupole/electrostatic field orbitrap high-resolution mass spectroscopy(Q-Orbitrap-HRMS) QuEChERS fish and fishery products nitroimidazole benzimidazoles |
引用本文:李蓉,杨璐齐,罗阳丹,张朋杰,高永清.QuEChERS/UPLC-Q-Orbitrap HRMS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[J].分析测试学报,2018,37(5):547-555. |
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