【摘要】 应用Qu ECh ERS前处理技术,建立了鸡肉和鸡肝中扎那米韦残留量的超高效液相色谱-串联质谱快速测定方法。样品经0.2 mol/L盐酸溶液-甲醇(1∶9)超声提取,离心后分取上清液,应用Qu ECh ERS净化。化合物采用NUCLEOSHELL HILIC(3.0 mm×100 mm,2.7μm)柱以5 mmol/L乙酸铵-0.2%甲酸溶液和乙腈为流动相梯度洗脱分离,电喷雾电离(ESI)正离子多反应监测模式(MRM)进行测定,标准曲线外标法定量。结果表明,扎那米韦在5~100 ng/m L范围内线性关系良好,相关系数(r)大于0.990;方法的定量下限(S/N=10)为10μg/kg。以鸡肉和鸡肝为基质,在10,20,100μg/kg加标水平下的平均回收率为80.5%~88.7%,相对标准偏差(RSD,n=6)为7.3%~11.8%,已应用于实际鸡肉样品的检测。该方法灵敏度高、重复性好、操作简单、快捷,适用于鸡肉组织中扎那米韦残留量的分析测定。更多还原

【Abstract】 A rapid method for the determination of zanamivir residues chicken tissues was developed using Qu ECh ERS approach coupled with ultra-performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS). After ultrasonically extracted with( 0. 2 mol / L) hydrochloric acid-methanol( 1 ∶ 9),the supernate was purified by Qu ECh ERS method. The separation was performed on a NUCLEOSHELLHILIC( 3. 0 mm × 100 mm,2. 7 μm) column by gradient elution using a mobile phase consisted of 5 mmol / L ammonium acetate( containing 0. 2% formic acid) and acetonitrile.The identification of zanamivir was carried out by MS / MS in positive electrospray ionization( ESI+)and multiple-reaction monitoring( MRM) mode,and the quantification was performed by the external standard calibration method. The results showed that the calibration curves were linear in the range of5- 100 ng / m L with correlation coefficients( r) greater than 0. 990. The limits of quantitation( LOQs,S / N = 10) of this method were 10. 0 μg / kg for the chicken muscle and liver. The average recoveries of zanamivir at three spiked levels of 10,20,100 μg / kg were in the range of 80. 5%- 88. 7% with relative standard deviations( RSDs,n = 6) of 7. 3%- 11. 8%. The method was applied in the determination of zanamivir residues in practical chickens. The developed method is simple, accurate,rapid,sensitive and efficient,and could be applied in the determination of zanamivir residues in chicken tissues.更多还原