QuEChERS-dSPE-UPLC-MS/MS筛查中药材地龙中41种兽药残留

QuEChERS -dSPE-UPLC-MS/MS for Rapid Determination of 41 Kinds of Veterinary Drug Residue in Pheretima

关键词:  QuEChERS  分散式固相萃取管  超高效液相色谱串联三重四极杆质谱法  动态多反应监测模式（d-MRM）  地龙  兽药残留  筛查

Key words:  QuEChERS  dispersed solid phase extraction  UPLC-MS/MS  d-MRM  Pheretima  veterinary drug residue  screen

摘要:

本文建立了基于超高效液相色谱串联三重四极杆质谱（UPLC-MS/MS）的动态多反应监测（d-MRM）模式快速筛查中药材地龙中7大类（喹诺酮类、磺胺类、糖皮质激素类、硝基咪唑类、抗病毒类、非甾体抗炎药、镇静剂）41种兽药残留的分析方法。样品采用QuEChERS提取， EMR-Lipid分散式固相萃取管 (EMR-Lipid dSPE) 进行净化，采用 d-MRM采集模式进行定性和定量检测，外标法定量，41种兽药测定在各自线性范围呈良好的线性关系，相关系数（R2）均大于0.9917，检出限为0.1000 ~ 3.105 μg/kg，定量限为0.3184 ~ 7.532 μg/kg，3个添加水平的回收率为70.1% ~ 119.7%，精密度为1.1%～6.3%。该方法前处理简单、重现性好、灵敏度高，适用于中药材地龙中41种兽药残留的快速筛查。

Abstract:

A method was established for rapid screening 41 kinds of veterinary drug residue in Pheretima based on dynamic model of multiple reaction monitoring (MRM) by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS) in this paper. The sample was extracted with quick、easy、cheap、effective、rugged and safe(QuEChERS), then purified with EMR-Lipid dispersed solid phase extraction (EMR-Lipid dSPE). The dynamic multiple reaction monitor(d-MRM) acquisition mode was used for qualitative and quantitative detection, and external standard method was used for quantitative detection.The analytes showed good linearities in corresponding concentration ranges with their correlation coefficients(R2) no less than 0.9917. The limit of detection were 0.1000 ~ 3.105 μg/kg, the limit of quantitative were 0.3184 ~ 7.532 μg/kg, the spiked recoveries for analytes at three spiked levels were in the range of 70.1% ~ 119.7%, the precision were 1.1% ~ 6.3%. The pretreatment method is simple, reproducible and sensitive, and suitable for the rapid screening of 41 kinds of veterinary drug residues in Pheretima.