| 摘要: |
| 采用超高效液相色谱-串联质谱法(UPLC-MS/MS),结合PRIME HLB快速通过式前处理技术,通过优化样品前处理及色谱-质谱条件,建立了同时提取、动态多反应监测(MRM)同时测定β-内酰胺类、抗病毒类、大环内酯类、喹诺酮类、四环素类、林可胺类、磺胺类、氯霉素类和氟虫腈及其代谢物共 9 类 38种药物残留的新方法。鸡蛋样品经80%(V/V)乙腈-水溶液(含0.02mol/L EDTA)提取后,PRIME HLB固相萃取柱净化,基质匹配外标法定量。38种药物在3个不同浓度水平下,平均回收率为71.4%～108.2%；相对标准偏差(RSD)为0.7%～8.1%；检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.01～1.0μg/kg和0.05～3.5μg/kg。本方法简便快速,灵敏可靠,适用于鸡蛋中药物多残留高通量快速检测分析。 |
| 关键词: PRIME HLB,超高效液相色谱串联质谱,残留,鸡蛋 |
| DOI： |
| 投稿时间：2019-01-07修订日期：2019-04-29 |
| 基金项目: |
|
| Rapid Detection of 38 Drug Residues in Eggs Based on PRIME HLB and Its Application in Risk Monitoring |
|
| (Shandong Provincial Veterinary Medicine Supervision Institute/Shandong Provincial Key Laboratory of Quality Safety Monitoring and Risk Assessment for Livestock and Poultry Products) |
| Abstract: |
| A method based on ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 38 drug residues, belonging to nine classes (β-Lactams, antiviral agents, macrolides, quinolones, tetracyclines, lincosamides, sulfonamides, chloramphenicols, fipronil and its metabolite), in eggs. This method was based on the new solid phase extraction column，PRiME HLB．The targeted compounds in eggs were extracted with acetonitrile /water (80:20, v/v) containing 0.02 mol/L EDTA，then through PRIME HLB，and the matrix-matching external standard method was used to quantify．The average recoveries of the 38 analytes ranged from 71.4% to 108.2%，and the relative standard deviation (RSD) in three different concentrations was 0.7%～8.1%． The limit of detection (LOD，S/N≥3) and quantification (LOQ，S/N≥10) were 0.01～1.0 μg/kg and 0.05～3.5 μg/kg，respectively． The method is simple，fast，sensitive and reliable，and is suitable for the rapid determination of drug residues in eggs. |
| Key words: UPLC-MS/MS residues egg |
