HPLC-MS-MS法快速筛查4种常见强极性除草剂

Rapid screening of four common highly polar herbicides by HPLC-MS-MS

目的建立一种高效液相色谱串联质谱快速筛查4种常见强亲水性除草剂的方法。方法4种强极性除草剂经亲水色谱Poroshell HILIC Plus柱(2.1mm×100mm,2.7μm)分离,以同一流动性B和酸性、碱性两种流动相A通过溶剂切换进行梯度洗脱,MRM正负模式进行检测。结果4种强极性除草剂在5~100ng/ml范围内线性关系良好(r^(2)>0.99),LOD为0.3~2ng/ml,LOQ为1~5ng/ml,空白血液添加目标化合物回收率为87%~104%,日内RSD为1.5%~3.8%,日间RSD为2.7%~5.1%。结论该方法无需衍生化,同时适用于4种常见除草剂的检测,将传统方法合二为一,更简便快捷,灵敏度和重现性符合一般毒物检验要求,并通过实际案件检验验证。

Objective A non-derivatized high-performance liquid chromatography-tandem mass spectrometry method was established for rapid screening of four common herbicides with strong hydrophilicity:paraquat,diquat,glyphosate and glufosinate-ammonium.Method The four highly polar herbicides were separated by a hydrophilic chromatography Poroshell HILIC Plus column.The same fluidity B and two acidic and alkaline mobile phases A were used for gradient elution through solvent switching.Negative multiple reaction monitoring mode for detection.Result The experimental results show that the four highly polar herbicides have a good linear relationship in the range of 5~100 ng/mL(r^(2)>0.99),the LOD is 0.3~2 ng/mL,the LOQ is 1~5 ng/mL,and the blank blood is recovered by adding the target compound.The rate is 87%~104%,the intra-day RSD is 1.5%~3.8%,and the intra-day RSD is 2.7%~5.1%.Conclusion The method does not require derivatization,and is suitable for the simultaneous detection of four common herbicides.It combines traditional methods into one,which is simpler and faster.The sensitivity and reproducibility meet the general toxicant inspection,and it has been verified by actual case inspections.