摘要
目的建立血液中啶虫脒和哒螨灵的液相色谱-串联质谱的检测方法。方法取0.5 m L血用1.0 m L乙腈沉淀蛋白,选用Kinetex~?2.6μm C18 100mm×2.1mm色谱柱,以乙腈(A相)和20m M乙酸铵+0.1%甲酸(B相)作为流动相进行梯度洗脱分离,采用液相色谱-串联质谱仪的电喷雾电离,正离子模式扫描,多反应监测模式(MRM)检测啶虫脒和哒螨灵,并用外标法定量。结果该方法可有效分离血中啶虫脒和哒螨灵,保留时间分别为1.06min和2.74min。血中啶虫脒和哒螨灵在0.5~100ng/m L范围内线性良好,回归方程分别为y=52753x+1024和y=98780x+3466,定量限为0.5ng/m L。啶虫脒和哒螨灵的回收率均在70%以上,精密度均小于10%。结论本文所建立方法简便、快速、有效,适用于血中啶虫脒和哒螨灵定性定量检测。
Objective To establish an assay of liquid chromatography in tandem with mass spectrometry for simultaneousdetermination of acetamiprid and pyridaben in blood samples.Methods Aliquots of0.5mL blood samples were used forthe analysis.Acetamiprid and pyridaben were extracted with1.0mL acetonitrile to precipitate protein.The separation wasperformed on a Kinetex?2.6μm-C18100mm×2.1mm analytical column by the Shmiadzu’s system of SIL-30AC highperformanceliquid chromatography.The running parameters were the flow rate of0.6mL/min,injection volume being3μL,column temperature at40℃.The mobile phases consisted of acetonitrile(mobile phase A)and water containing20mM ammoniumacetate plus0.1%formic acid(mobile phase B),flowing under gradient elution.The MS/MS analysis was conductedwith AB QTRAP6500tandem mass spectrometry at the conditions of positive electrospray ionization mode(ESI+),multiplereaction monitoring(MRM)and external standard for quantification.Results Acetamiprid and pyridaben were well separatedin blood samples with their respective retention time of1.06min and2.74min.Calibration curves for the two chemicalswere linear within the range of0.5~100ng/mL,with their regression equations as y=52753x+1024and y=98790x+3466.Forboth acetamiprid and pyridaben,the limits of quantitation were0.5ng/mL,recoveries more than70%,and relative standarddeviation showing less than10%.Conclusion This method is simple,rapid and effective,suitable for determination ofacetamiprid and pyridaben in blood samples.
作者
康伟
周拓
陈愉
贺纪明
刘俊
吴开封
KANG Wei;ZHOU Tuo;CHEN Yu;HE Jiming;LIU Jun;WU Kaifeng(Ningbo Institute of Forensic Science, Ningbo 315000, Zhejiang, China)
出处
《刑事技术》
2017年第5期379-381,共3页
Forensic Science and Technology
