超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速检测茶叶中草甘膦、草铵膦及其代谢物残留

Rapid determination of glyphosate, glufosinate-ammonium and their metabolite residues in tea by ultra performance liquid chromatography-quadrupole electrostatic field orbital trap high resolution mass spectrometry

中文关键词:  茶叶  超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法  草甘膦  草铵膦  代谢物  通过式固相萃取

英文关键词:tea  ultra performance liquid chromatography-quadrupole electrostatic field orbital trap high resolution mass spectrometry  glyphosate  glufosinate-ammonium  metabolite residues  pass-through solid phase extraction

中文摘要:

      目的 建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(ultra performance liquid chromatography-quadrupole electrostatic field orbital trap high resolution mass spectrometry, UPLC-Q-Orbitrap HRMS)测定茶叶中草甘膦、草铵膦及代谢物的的快速分析方法。方法 称取1.00 g茶叶样品, 加入20 mL含1%甲酸的甲醇-水(1:1, V:V)提取液, 超声提取5 min, 4500 r/min离心5 min, 经Oasis PRiME HLB固相萃取柱通过式净化, 并通过超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法对样品进行测定。结果 茶叶中草甘膦、草铵膦及代谢物在5.0~50 ng/mL的范围内, 线性关系良好(r2＞0.999), 平均回收率在83.7%~92.2%之间, 相对标准偏差低于10%, 检出限为0.02 mg/kg, 定量限为0.05 mg/kg。结论 此方法前处理简便快速, 且准确性好、灵敏度高, 可实现茶叶中草甘膦、草铵膦及其代谢物的快速筛查。

英文摘要:

      Objective To establish a method for the determination of glyphosate, glufosinate-ammonium and their metabolite residues in tea by ultra performance liquid chromatography-quadrupole electrostatic field orbital trap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). Methods 1.00 g tea sample was weighed, 20 mL methanol water (1:1, V:V) extraction solution containing 1% formic acid was added, ultrasonic extraction was performed for 5 min, and centrifugation was performed at 4500 r/min for 5 min. The sample was purified by Oasis PRiME HLB solid phase extraction column, and determined by UPLC-Q-Orbitrap HRMS. Results The linear relationship between glyphosate, glufosinate-ammonium and their metabolite residues in tea was good in the range of 5.0?50 ng/mL (r2>0.999), the average recoveries were between 83.7%?92.2%, the relative standard deviation (RSD) was less than 10%, the limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitative (LOQ) was 0.05 mg/kg. Concluson This method is simple, rapid, accurate and sensitive, which can realize the rapid screening of glyphosate, glyphosate-ammonium and their metabolite residues in tea.