基于HPLC-MS/MS对海博麦布中对甲苯胺、对氟苯胺、邻氟苯胺的残留检测研究

Residual detection of 4-aminotoluene,4-fluoroaniline and 2-fluoroaniline in hybutimibe by HPLC-MS/MS

基于HPLC-MS/MS法建立海博麦布中对甲苯胺、对氟苯胺、邻氟苯胺的检测方法。采用高效液相色谱进行分离,以Waters ACQUITY UPLC^(?)BEH C_(18)(2.1 mm×100.0 mm,1.7μm)为色谱柱,以0.1%甲酸溶液和甲醇为流动相,梯度洗脱;以三重四极杆质谱为检测器,质谱采用电喷雾离子源、正离子、多反应监测模式(MRM)采集数据。结果显示,对甲苯胺、对氟苯胺、邻氟苯胺在1.0000~20.0000 ng/L范围内线性关系良好,相关系数(r)为0.9975~0.9999;方法检出限为0.33 mg/kg,定量限为1.00 mg/kg;方法加样回收率为85%~95%。本方法建立了海博麦布中对甲苯胺、对氟苯胺、邻氟苯胺的检测方法。该方法操作简单,线性关系良好,检出限低,回收率高,可为海博麦布制备工艺中对甲苯胺、对氟苯胺、邻氟苯胺的质量控制提供技术支持。

A high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) method was established to determinate the residues of 4-aminotoluene,4-fluoroaniline and 2-fluoroaniline in hybutimibe.The compounds were separated by high performance liquid chromatography with Waters ACQUITY UPLC~?BEH C_(18)(2.1 mm×100.0 mm,1.7μm) column.0.1%formic acid solution was used as the mobile phase A and methanol as the mobile phase B in gradient elution.The detector was triple quadrupole mass spectrometry.The MS data for the compounds were collected by positive ion electrospray ionization (ESI) using multi reaction monitoring mode (MRM)The linear ranges of 4-aminotoluene,4-fluoroaniline and 2-fluoroaniline were 1.000 0-20.000 0 ng/L,correlation coefficients (r) were 0.997 5-0.999 9.The detection limit concentrations were 0.33 mg/kg,and the quantification limit concentrations were 1.00 mg/kg.The method recovery rates were 85%-95%.The method is simple with good linear relationship,low detection limit and high recovery rate,which provide a technical support for the quality control of4-aminotoluene,4-fluoroaniline and 2-fluoroaniline in hybutimibe.