高效液相色谱-串联质谱法测定猪组织中泰地罗新残留  

Determination of tildipirosin residues in swine tissues by high performance liquid chromatography-tandem mass spectrometry

作　　者：王文湘[1] 闫超群 华成云 李国基 王波[1] 顾欣[2] 曹莹[2] 黄士新[2] 黄显会[1] WANG Wenxiang;YAN Chaoqun;HUA Chengyun;LI Guoji;WANG Bo;GU Xin;CAO Ying;HUANG Shixin;HUANG Xianhui(College of Veterinary Medicine,South China Agricultural University/Guangdong Provincial Key Laboratory for Veterinary Pharmaceutics Development and Safety Evaluation,Guangzhou 510642,China;Shanghai Animal Disease Prevention and Control Center,Shanghai 201103,China)

机构地区：[1]华南农业大学兽医学院/广东省兽药研制与安全评价重点实验室,广东广州510642 [2]上海市动物疫病预防控制中心,上海201103

出　　处：《华南农业大学学报》2018年第6期32-38,共7页Journal of South China Agricultural University

基　　金："十三五"国家重点研发计划(2016YFD0501306)

摘　　要：【目的】建立适用于猪组织中泰地罗新残留检测的高效液相色谱-串联质谱法。【方法】猪组织(肌肉、肝脏、肾脏和皮脂)样品经0.1 mol·L^(–1)磷酸二氢钾溶液提取,上清液采用HLB固相萃取柱浓缩净化,Phenomenex Luna Omega C18色谱柱梯度洗脱,采用电喷雾正离子扫描和多反应监测(MRM)模式对泰地罗新进行分析,采用基质匹配法对泰地罗新含量进行标准校正。【结果】泰地罗新添加剂量在肌肉中25~2 400 ng·g^(-1)、肝脏中25~2 500 ng·g^(-1)、肾脏中25~2 000 ng·g^(-1)和皮脂中25~1 600 ng·g^(-1)的范围内,与特征离子峰面积呈良好的线性关系(r2≥0.99)。猪组织添加泰地罗新样品中肌肉、肝脏、肾脏和皮脂的检测限均为10 ng·g^(-1),定量限均为25 ng·g^(-1)。对猪组织在定量限、1/2MRL、MRL、2MRL这4个剂量下进行泰地罗新的添加回收试验,各组织中的批内平均回收率为85.6%~105.0%,批内回收率相对标准偏差2.3%~9.5%,批间回收率相对标准偏差4.7%~7.6%。【结论】该方法简单易行,灵敏度高且特异性强,可用于猪组织中泰地罗新残留量的分析测定。【Objective】To establish a reliable HPLC-MS/MS(High performance liquid chromatographytandem mass spectrometry)method suitable for determing tildipirosin residues in swine tissues.【Method】Swine tissue samples,including muscle,liver,kidney and skin-fat were extracted with 0.1 mol·L–1 KH2PO4 buffer solution.The supernatant fluids were enriched and purified using HLB solid-phase extraction column,and gradiently eluted by Phenomenex Luna Omega C18 liquid chromatography column.The analytes were then detected using triple-quadrupole mass spectrometry in positive electrospray ionization and multiple reaction monitoring(MRM)mode.The matrix-matched method was used to calibrate tildipirosin content.【Result】Tildipirosin contents presented good linear relationships(r2>0.99)with characteristicion peak area in the ranges of 25–2 400 ng·g–1 in muscle,25–2 500 ng·g–1 in liver,25–2 000 ng·g–1 in kidney and 25–1 600 ng·g–1 in skin-fat.All the limits of detection and quantitation in muscle,liver,kidney and skin-fat samples added tildipirosin were 10 and 25 ng·g–1,respectively.The recovery experiments of tildipirosin in swine tissues were setted in four dosage levels,including limit of quantitation,1/2 maximum residue limit(MRL),MRL and 2MRL,and the mean intra-batch recoveries of tildipirosin in all analytes ranged from 85.6%to 105.0%.The relative standard deviations of intra-batch and inter-batch recoveries were in the ranges of 2.3%–9.5%and 4.7%–7.6%,respectively.【Conclusion】The established method is simple,practicable,and with high sensitivity and specificity.It can be applied to determine tildipirosin residues in swine tissues.

关 键 词：猪组织 高效液相色谱–串联质谱 泰地罗新 残留 

分 类 号：S859.7[农业科学—临床兽医学]