分散固相萃取结合超高效液相色谱-串联高分辨质谱法快速测定羊乳中磺胺类药物

Rapid determination of sulfonamides in goat milk by dispersive solid phase extraction combined with ultra performance liquid chromatography tandem high resolution mass spectrometry

中文关键词:  分散固相萃取  超高效液相色谱-串联高分辨质谱法  多孔石墨烯  多壁碳纳米管  羊乳  磺胺

英文关键词:dispersive solid phase extraction  ultra performance liquid chromatography-tandem high resolution mass spectrometry  porous graphene  multi walled carbon nanotubes  goat milk  sulfonamides

中文摘要:

      目的 建立基于多孔石墨烯复合多壁碳纳米管纳米材料(multi walled carbon nanotubes-porous grapheme, MWCNTs@PG)的分散固相萃取结合超高效液相色谱-串联高分辨质谱法(ultra performance liquid chromatography tandem-high resolution mass spectrometry, UPLC-HRMS)快速测定羊乳中10种磺胺类药物的分析方法。方法 样品经QuEChERS处理, 分散固相萃取后(dispersive solid phase extraction, d-SPE)采用C18色谱柱分离, 正离子模式下高分辨数据依赖采集。研究了吸附剂种类、pH、洗脱溶剂种类、吸附剂用量、洗脱溶剂体积、吸附时间对磺胺提取效率与检测准确性的影响。结果 10种磺胺物质在各自的线性范围内的相关系数均大于0.99, 检出限为0.01~0.25 μg/kg, 回收率和精密度分别为75%~109%和0.6%~9.3%。结论 基于MWCNTs@PG分散固相萃取对羊乳中磺胺药物有较高的回收率和净化效果, 超高效液相色谱串联高分辨质谱法可实现快速分离、准确定性和精准定量, 适合于复杂基质中兽药残留的快速准确分析。

英文摘要:

      Objective To establish a method for the rapid determination of 10 kinds of sulfonamides in goat milk by dispersive solid phase extraction based on multi walled carbon nanotubes-porous grapheme (MWCNTs@PG) combined with ultra performance liquid chromatography-tandem high resolution mass spectrometry (UPLC-HRMS). Methods The sample was pretreated by QuEChERS followed by dispersive solid phase extraction (d-SPE) and separated by C18 chromatographic column, and high resolution data dependent acquisition under positive ion mode. The effects of adsorbent type, pH, elution solvent type, adsorbent amount, volume of elution solvent and adsorption time on the extraction efficiency and detection accuracy of sulfonamides were studied. Results The correlation coefficients of 10 kinds of sulfonamides in their respective linear ranges were greater than 0.99, the detection limits were 0.01?0.25 μg/kg, the recoveries and precisions were 75%?109% and 0.6%-9.3% respectively. Conclusion The dispersive solid phase extraction based on MWCNTs@PG has high recoveries and purification effects on sulfonamides in goat milk. UPLC-HRMS can achieve rapid separation, accurate qualitative and quantitative analysis, which is suitable for rapid and accurate analysis of veterinary drug residues in complex matrixes.