超分子溶剂分散液液微萃取/超高效液相色谱-串联质谱法测定鱼血中13种硝基咪唑类药物残留
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摘要
建立了一种基于超分子溶剂分散液液微萃取技术测定鱼血中13种硝基咪唑类药物的超高效液相色谱-串联质谱方法。样品用正辛醇、四氢呋喃和水形成的超分子溶剂萃取,以乙腈-水为流动相进行梯度洗脱,采用Waters ACQUITY UPLC BEH C_(18)(2.1 mm×50 mm×1.7μm)色谱柱分离。在电喷雾正离子模式下,采用多反应监测模式进行定性及定量分析。结果表明,13种硝基咪唑类药物在各自范围内线性关系良好,相关系数(r~2)大于0.998,检出限为0.05～0.2μg/L,定量下限为0.1～0.5μg/L。在低、中、高3个加标水平下,13种硝基咪唑类药物的平均回收率为88.4%～105%,相对标准偏差(n=6)为4.3%～11%。该方法简便快速、准确可靠,可用于鱼血中硝基咪唑类药物残留的分析检测。
A novel method was developed for the determination of thirteen nitroimidazoles in fish blood by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with supramolecular solvent-based dispersive liquid-liquid microextraction.The target compounds in fish blood were extracted with a supramolecular solvent consisted of octanol,tetrahydrofuran and water.The analytes were separated on a Waters ACQUITY UPLC BEH C_(18) column(2.1 mm×50 mm×1.7 μm) by gradient elution with acetonitrile-water as mobile phases.The qualitative and quantitative analyses were conducted by electrospray ionization mass spectrometry in positive ion mode under multiple reaction monitoring(MRM) mode.Experimental results demonstrated that good linearities for the analytes were observed in their respective concentration ranges with correlation coefficients(r~2) larger than 0.998.The limits of detection(LOD) and the limits of quantitation(LOQ) were in the ranges of 0.05-0.2 μg/L and 0.1-0.5 μg/L,respectively.Recoveries for 13 nitroimidazoles at three spiked levels ranged from 88.4% to 105% with relative standard deviations(n=6) of 4.3%-11%.The method was simple,rapid,accurate and reliable,and could be used for the analysis of nitroimidazole residues in fish blood samples.
A novel method was developed for the determination of thirteen nitroimidazoles in fish blood by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with supramolecular solvent-based dispersive liquid-liquid microextraction.The target compounds in fish blood were extracted with a supramolecular solvent consisted of octanol,tetrahydrofuran and water.The analytes were separated on a Waters ACQUITY UPLC BEH C_(18) column(2.1 mm×50 mm×1.7 μm) by gradient elution with acetonitrile-water as mobile phases.The qualitative and quantitative analyses were conducted by electrospray ionization mass spectrometry in positive ion mode under multiple reaction monitoring(MRM) mode.Experimental results demonstrated that good linearities for the analytes were observed in their respective concentration ranges with correlation coefficients(r~2) larger than 0.998.The limits of detection(LOD) and the limits of quantitation(LOQ) were in the ranges of 0.05-0.2 μg/L and 0.1-0.5 μg/L,respectively.Recoveries for 13 nitroimidazoles at three spiked levels ranged from 88.4% to 105% with relative standard deviations(n=6) of 4.3%-11%.The method was simple,rapid,accurate and reliable,and could be used for the analysis of nitroimidazole residues in fish blood samples.
引文
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[4] Qin G X,Xu W Y,Ai X H,Tang G P,Cui J,Li X H,Yuan K P.J.Northwest A & F Univ.:Nat.Sci.Ed.(秦改晓,徐文彦,艾晓辉,唐国盘,崔锦,李向辉,袁科平.西北农林科技大学学报:自然科学版),2012,40(8):13-20.
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