超高效液相色谱-三重四极杆/复合线性离子阱质谱法快速测定动物源性食品中5种硝基咪唑类药物残留

Fast determination of five nitroimidazoles drug residue in animal-derived foods by ultraperformance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry

目的 采用通过式净化柱-超高效液相色谱-三重四级杆/复合线性离子阱质谱技术,建立了动物源性食品中5种硝基咪唑类药物残留的快速确证检测方法。方法 样品经1%甲酸-乙腈溶液提取后离心,上清液直接通过PRiME HLB柱净化,然后进入超高效液相色谱-三重四极杆/复合线性离子阱质谱(UPLC-QTRAP MS)进行分析。对净化条件、流动相、色谱柱等进行了优化。确定以PRiME HLB柱净化,Acquity BEH C18柱为分析柱,0.1%甲酸水和乙腈溶液做为流动相,电喷雾正离子模式下多反应监测-触发增强子离子扫描(MRM-IDA-EPI)方式检测,同位素内标法定量。结果 方法的定量限为0.30~0.80μg/kg。蛋、肉及水产中加标回收率范围为73.2%~115.2%,相对标准偏差为3.2%~9.3%。结论 该方法快速、灵敏、准确,适用于动物源性食品中硝基咪唑类药物残留的检测,可应用于大批量样品的筛查及确证。

Objective A fast confirmation method was developed for the determination of five nitroimidazoles drug residues in animal-derived foods by ultraperformance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry coupled with solid phase extraction.Methods The samples were extracted with 1% formic acid-acetonitrile and then centrifuged.The supernatant was directly purified by solid phase extraction based on PRIME HLB cartridge,and then determined by ultraperformance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry.The purification condition,mobile phase and chromatographic column were optimized.Under the optimal conditions,the sample was purified by prime HLB column and analyzed by BEH C18 column with 0.1% formic acid-water and acetonitrile as mobile phase.The five nitroimidazoles were detected with positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring-information-dependent acquisition-enhanced product ion(MRM-IDA-EPI) mode,and quantified by isotopically labeled internal standard.Results The limits of quantitation were from 0.30 to 0.80 μg/kg.The average recovery rates of the 5 nitroimidazoles were 73.2%-115.2% with relative standard deviations of 3.2%-9.3%(n=6).Conclusion The developed method is rapid,sensitive,accurate and suitable for the detection of nitroimidazole residues in animal-derived foods.The method can be used for screening and confirmation of samples in large quantities.