高效液相色谱-串联质谱法检测鸡组织及鸡蛋中新型兽药氟雷拉纳残留

Determination of Residues of the Novel Veterinary Drug Fluralaner in Chicken Tissues and Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry

基于高效液相色谱-串联质谱法建立鸡组织(鸡肉、鸡肝、鸡皮和鸡肾)及鸡蛋中新型兽药氟雷拉纳残留的检测方法。将低(0.10 mg/kg)、中(0.25 mg/kg)、高(0.50 mg/kg)剂量氟雷拉纳分2次灌胃(间隔7 d)白羽母鸡后获得阳性动物样品。样品经乙腈提取、PRiME HLB固相萃取小柱净化后,以甲醇和5 mmol/L甲酸铵溶液为流动相,Eclipse Plus C18色谱柱为分离柱进行梯度洗脱,电喷雾负离子模式电离,在多反应监测模式下检测,绘制基质匹配校准曲线,外标法定量。结果表明:氟雷拉纳在0~200 ng/mL质量浓度范围内具有良好的线性关系,相关系数(R^(2))>0.99,方法检出限为2.0μg/kg,定量限为5.0μg/kg;在5、15、50μg/kg加标水平下,鸡组织(鸡肉、鸡肝、鸡皮、鸡肾)和鸡蛋中氟雷拉纳的平均加标回收率为81.2%~99.1%,相对标准偏差为1.29%~7.86%(n=6)。该方法成功应用于阳性动物样品中氟雷拉纳残留量的检测。综上,该方法简便、快速、灵敏,适用于鸡组织及鸡蛋中氟雷拉纳兽药残留的检测。

This study established a method for the determination of fluralaner residues in chicken tissues(meat,liver,skin and kidney)and eggs by high performance liquid chromatography-tandem mass spectrometry.Positive animal samples were obtained from white-feathered laying hens orally administered of low(0.10 mg/kg),medium(0.25 mg/kg)and high(0.50 mg/kg)doses of fluralaner(in two fractions,7 d apart).Samples were extracted with acetonitrile and purified by solid phase extraction on a PRiME HLB column.The target analyte was separated on an Eclipse Plus C18 column with gradient elution using a mobile phase consisting of methanol and 5 mmol/L ammonium formate solution and analyzed using electrospray ionization in the negative ion mode with multiple reaction monitoring(MRM).A matrix-matched calibration curve was prepared and the external standard method was used for quantification under the optimal conditions.The calibration curve showed good linearity in the concentration range of 0–200 ng/mL with correlation coefficient(R^(2))greater than 0.99.The limit of detection(LOD)and the limit of quantification(LOQ)were 2.0 and 5.0μg/kg,respectively.The recoveries of added fluralaner from chicken meat,eggs,liver,skin and kidney were 81.2%–99.1%with relative standard deviations(RSDs)of 1.29%–7.86%at spiked levels of 5,15 and 50μg/kg(n=6).The method is simple,rapid,sensitive,and has been successfully applied for the determination of fluralaner residues in medicated chicken samples.