QuEChERS方法结合超高效液相色谱-串联质谱法快速检测鸡肉组织中扎那米韦药物的残留量  

Rapid Determination of Zanamivir Residues in Chicken Tissues Using Qu ECh ERS Combined with Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：任明兴 刘正才[2] 唐寰宇[2] 杨方[2] 林永辉[2] 苏芝娇[2] 董文洪 

机构地区：[1]绍兴出入境检验检疫局,浙江绍兴312000 [2]福建出入境检验检疫局,福建福州350001

出　　处：《分析测试学报》2016年第7期854-858,共5页Journal of Instrumental Analysis

基　　金：国家质检总局科技项目(2014IK110)

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。A rapid method for the determination of zanamivir residues chicken tissues was developed using QuEChERS 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 QuEChERS method. The separation was performed on a NUCLEOSHELL HILIC（3.0 mm× 100 mm, 2.7 μm） column by gradient elution using a mo- bile 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 of 5 - 100 ng/mL 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 deter- mination 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 inchicken tissues.

关 键 词：QU ECH ERS方法 超高效液相色谱-串联质谱法 扎那米韦 残留量 鸡肉组织 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]