超高效液相色谱-四极杆/静电场轨道阱高分辨质谱测定豆类杂粮中53种农药残留

Determination of 53 kinds of pesticide residues in coarse cereals by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

中文关键词:  超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法  杂粮  农药残留

英文关键词:ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry  coarse cereals  pesticide residues

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测定杂粮中53种农药残留的分析方法。方法 杂粮样品采用乙腈提取, 经MgSO4、乙二胺-N-丙基硅烷化硅胶、C18混合净化剂净化, CAPCELL CORE AQ柱(150 mm×3 mm, 2.7 μm)分离, 以5 mmol/L甲酸铵水溶液(含0.1%甲酸, V:V)-5 mmol/L甲酸铵甲醇溶液(含0.1％甲酸,V:V)为流动相, 在全扫描和自动触发二级质谱(Full MS/dd-MS2)模式下采集数据。结果 53种目标物在各自范围内线性关系良好, 相关系数(r2)均大于0.99, 定量限为1~10 μg/kg, 平均回收率为73.8%~119.7%, 相对标准偏差为0.7%~12.1%。结论 该法操作简便, 灵敏, 适用于杂粮中53种农药残留的定性、定量筛查。

英文摘要:

      Objective To establish a method for determination of 53 pesticide residues in coarse cereals by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry. Methods The coarse cereals samples were extracted by acetonitrile, purified by a mixed sorbent of MgSO4, primary secondary amine and C18, and separated with a CAPCELL CORE AQ column (150 mm× 3 mm, 2.7 μm) using water [containing 0.1% (V:V) formic acid and 5 mmol/L ammonium formate] and methanol [containing 0.1％(V:V) formic acid and 5 mmol/L ammonium formate] as mobile phase by gradient elution. The data were acquired in full scan and automatically triggered secondary mass spectrometry (Full MS/dd-MS2) modes. Results The calibration curves were linear with correlation coefficients greater than 0.99, the limits of quantitation were 1–10 μg /kg, and the recoveries were 73.8%–119.7%, with the relative standard deviations of 0.7%–12.1%. Conclusions This method is simple and sensitive, which can be suitable for the qualitative determination and quantitative analysis of 53 pesticide residue in coarse cereals.