高效液相色谱-串联质谱法检测猪可食性组织中加米霉素残留

Determination of Gamithromycin Residues in Swine Edible Tissues by High Performance Liquid Chromatography-Tandem Mass Spectrometry

为了建立一种可靠、灵敏的检测猪可食性组织中加米霉素残留量的高效液相色谱-串联质谱方法,本试验将猪组织(肌肉、肝脏、脂肪和肾脏)经绞碎、均质后,用乙腈提取,乙腈饱和正己烷去脂,固相萃取柱净化,Kinetex C18色谱柱梯度洗脱,在电喷雾正离子下以多反应监测模式检测,内标法定量。结果显示,该方法的检测限和定量限分别为3μg/kg和5μg/kg;加米霉素在5~1000μg/kg浓度范围内,峰面积与浓度的线性关系良好;猪肌肉、肝脏和脂肪在5、50、100μg/kg和200μg/kg四个添加浓度的平均回收率为70.20%~90.75%,批间变异系数≤11.94%;猪肾脏在5、150、300μg/kg和600μg/kg四个添加浓度的平均回收率为66.69%~87.46%,批间变异系数≤9.95%。结果表明该方法灵敏、准确,可满足兽药残留检测的要求。

This study aimed to develop and optimize a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)for reliable and sensitive determination of gamithromycin residues in swine edible tissues.Swine tissues(muscle,liver,fat and kidney)were minced and homogenized,then extracted with acetonitrile,degreased with acetonitrile saturated n-hexane and purified by solid phase extraction column.The purified samples were separated chromatographically on a Kinetex C18 column with gradient elution,detected by multiple reaction monitoring mode under electrospray positive ions and quantified by internal standard method.The results showed that the limits of detection and quantification were 3μg/kg and 5μg/kg,respectively;the method had a good linearity at the range of 5-1000μg/kg;the average recoveries of swine tissues(muscle,liver and fat)were 70.20%-90.75%,and the inter-assay coefficients of variation was less than or equal to 11.94%at the concentration of 5,50,100μg/kg and 200μg/kg;the average recoveries of swine kidney were 66.69%-87.46%,and the inter-assay coefficients of variation was less than or equal to 9.95%at the concentration of 5,150,300μg/kg and 600μg/kg.This sensitive and precise method amply meets the requirements of veterinary drug residue detection.