超滤管净化/高效液相色谱-串联质谱法测定动物源食品中喹诺酮类药物残留

Determination of Quinolones Residues in Animal-originated Foodstuffs by Ultrafiltration Tube Cleaning and High Performance Liquid Chromatography- Tandem Mass Spectrometry

建立了超滤管净化技术结合高效液相色谱-串联质谱同时测定动物源食品中10种喹诺酮类药物残留的新方法。样品经酸化乙腈提取后,采用50 m L Millipore超滤管（截留分子量3 k D）净化,离心液氮吹复溶后,经Waters Xbridge C18色谱柱进行分离,以0.1%甲酸-乙腈作为流动相进行梯度洗脱,电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测,外标法定量。结果表明,10种喹诺酮类药物在5.0~100μg/kg浓度范围内线性关系良好,方法的检出限为0.15~0.75μg/kg,定量下限为0.49~2.59μg/kg,在5.0,10,50μg/kg 3个加标水平下的回收率为71.4%~85.9%,相对标准偏差（n=6）为3.9%~10.7%。方法简便快速、灵敏度高、重复性好,可用于动物源食品中10种喹诺酮类药物残留的快速确证和定量分析。

A new method was established for the simultaneous determination of 10 quinolone （QN） residues in animal-originated foodstuffs by ultrafiltration tube cleaning with high performance liquid chromatography- tandem mass spectrometry （HPLC -MS/MS）. After extraction with acetonitrile （ containing 1% acetic acid）, the extract was purified with 50 mL Millipore ultrafiltration tube （ Mo- lecular Weight Cut- Off, MWCO： 3 kD）, and then the centrifugal liquid was evaporated to dryness under a stream of nitrogen, and redissolved. The analytes were separated on a Waters Xbridge C18 column using 0. 1% formic acid - acetonitrile as mobile phase. The identification and quantification of 10 quinolone residues were carried out under positive electrospray ionization （ESI ＋） in multiple reac- tion monitoring （MRM） mode, the quantification analysis was performed by the external standard method. The calibration curves showed good linearities in the range of 5.0 - 100 μg/kg for all QNs. The limits of detection for all QNs were in the range of 0. 15 -0. 75 μg/kg, and the limits of quanti- tation were 0. 49 - 2. 59 μg/kg. The recoveries of these analytes varied from 71.4% to 85.9% at spiked levels of 5.0, 10, 50 μg/kg, with relative standard deviations of 3.9% - 10. 7%. This method was simple, rapid, sensitive and reproducible, and could be applied in the determination of 10 quinolone residues in animal-originated foodstuffs.