PRiME HLB-超高效液相色谱-串联质谱法测定禽蛋中氯羟吡啶残留量

Determination of clopidol residues in poultry eggs by PRiME HLB-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  氯羟吡啶  禽蛋  PRiME HLB固相萃取  超高效液相色谱-串联质谱法

英文关键词:clopidol  poultry eggs  PRiME HLB solid phase extration  ultra performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立PRiME HLB净化技术结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测禽蛋中氯羟吡啶残留的测定方法。方法 以90%乙腈水溶液作为提取液, PRiME HLB固相萃取柱净化, C18色谱柱分离, 多反应监测(multiple reaction monitoring, MRM)模式下正离子模式扫描, UPLC-MS/MS进行分析。结果 氯羟吡啶在0.5~50.0 μg/kg范围内线性关系良好(r2≥0.9984), 方法检出限和定量限分别为0.5 μg/kg和1.0 μg/kg。在鸡蛋、鸭蛋、鸽蛋中加标回收率在88.4~95.8%之间, 相对标准偏差(relative standard deviations, RSDs) (n=6)在6.0%~12.7%之间。结论 本方法准确度、灵敏度高, 可用于禽蛋中氯羟吡啶的测定。

英文摘要:

      Objective To establish a method for the determination of clopidol residues in poultry eggs by PRiME HLB purification technique combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The extraction was carried out with 90% acetonitrile aqueous solution, and the PRiME HLB solid-phase extraction column was used for purification. The separation was performed on a C18 chromatographic column, and the analysis was conducted by scanning in positive ion mode under multiple reaction monitoring (MRM) mode with an UPLC-MS/MS. Results The relationships of clopidol were good within the range of 0.5–50.0 μg/kg (r2≥0.9984). The limits of detection and the limits of quantitation were 0.5 μg/kg and 1.0 μg/kg, respectively. The recoveries rate of adding standard in eggs, duck eggs and pigeon eggs were between 88.4% and 95.8%, and the relative standard deviations (RSDs) (n=6) were 6.0%–12.7%. Conclusion This method has high accuracy and sensitivity, and can be used for the determination of clopidol in poultry eggs.