固相萃取-高效液相色谱-串联质谱法同时检测鸡蛋及其制品中8种兽药残留

Simultaneous determination of 8 kinds of veterinary drug residues in eggs and their products by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  固相萃取  高效液相色谱-串联质谱法  鸡蛋  兽药残留

英文关键词:solid phase extraction  high performance liquid chromatography-tandem mass spectrometry  egg  veterinary drug residues

中文摘要:

      目的 建立一种快速、高效的固相萃取-高效液相色谱-串联质谱法同时测定鸡蛋及其制品中的甲硝唑、地美硝唑、氯霉素、氟苯尼考、甲砜霉素、尼卡巴嗪、金刚烷胺和灭蝇胺8种兽药的分析方法。方法 样品前处理采用80%乙腈(含0.1%甲酸)提取, 经PRiME HLB小柱净化后检测。以乙腈-0.05%甲酸为流动相, 在质谱检测器的多反应监测模式下以外标法定量。结果 8种兽药组分在1.0~200.0 ng/mL浓度范围内线性关系良好, 相关系数(r2)为0.9982~0.9999, 检出限范围为0.3~5.0 μg/kg, 定量限范围为1.0~10.0 μg/kg。加标实验分别添加低、中、高的3个水平浓度, 加标回收率达到82.1%~96.2%，相对标准偏差为2.13%~5.97% (n=5)。结论 该方法具有前处理简单、灵敏度高和检测速度快的优点, 适用于鸡蛋及其制品中8种兽药组分的同时监测和分析。

英文摘要:

      Objective To establish a rapid and efficient method for simultaneous determination of 8 kinds of veterinary drugs, including metronidazole, dimenazole, chloramphenicol, florfenicol, thiamphenicol, nicarbazine, amantadine and cyromazine in eggs and their products by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with 80% acetonitrile (containing 0.1% formic acid) for pretreatment, and purified on a PRiME HLB column for detection. Acetonitrile-0.05% formic acid was used as mobile phase and quantified by external standard method under the multi reaction monitoring mode of mass spectrometry detector. Results The linear relationships of 8 kinds of veterinary drugs components were good within the range of 1.0?200.0 ng/mL, with the correlation coefficients (r2) of 0.9982?0.9999, the limits of detection were 0.3?5.0 μg/kg, and the limits of quantitation were 1.0?10.0 μg/kg. In the spiked assay, low, medium and high concentrations were added, the recoveries were in the range of 82.1%?96.2%, and the RSD were 2.13%-5.97% (n=5). Conclusion This method has the advantages of simple pretreatment, high sensitivity and fast detection speed, and is suitable for the simultaneous monitoring and analysis of 8 kinds of veterinary drugs components in eggs and their products.