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
和燕玲 1杨荷友 1吴春艳 2潘妮娜 1李于西 1邱卫晓 1赵燕 1苟金霞 3邵伍军4
作者信息
- 1. 浙江海正药业股份有限公司,浙江台州 318000
- 2. 台州科技职业学院,浙江台州 318000
- 3. 浙江博锐生物制药有限公司,浙江台州 318000
- 4. 浙江海正药业股份有限公司,浙江台州 318000;台州科技职业学院,浙江台州 318000
- 折叠
摘要
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 C18(2.1 mm×100.0 mm,1.7 μm)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0.997 5～0.999 9;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.
Abstract
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 C18(2.1 mm×100.0 mm,1.7 μm)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 of 4-aminotoluene,4-fluoroaniline and 2-fluoroaniline in hybutimibe.
关键词
高效液相色谱/三重四极杆质谱/对甲苯胺/对氟苯胺/邻氟苯胺/残留检测Key words
high performance liquid chromatography/triple quadrupole mass spectrometry/4-aminotoluene/4-fluoroaniline/2-fluoroaniline/residual research引用本文复制引用
基金项目
浙江省2023年度高校国内访问工程师校企合作项目(FG2023323)
出版年
2024
国家科技期刊平台
NSTL
万方数据