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Determination of 24 Pesticides in Putrefied Blood by Ultra Performance Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry |
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DOI: |
KeyWord:ultra performance liquid chromatography coupled with quadrupole-time of flight-mass spectrometry( UPLC-Q-TOF-MS) pesticide putrefied blood |
Author | Institution |
GUO Zhen,CHANG Jing,YANG Rui-qin*,LUAN Yu-jing,WANG Fang-lin,YU Zhong-shan |
1.中国人民公安大学刑事科学技术学院,2.公安部物证鉴定中心 |
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Abstract: |
An analytical method was established for the simultaneous determination of 24 pesticides in putrefied blood by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS).The QuEChERS(Quick,Easy,Cheap,Effective,Rugged,and Safe) method was used for sample preparation.The analytes were extracted with acetonitrile-waters(4∶1) by supersonic, dehydrated by adding anhydrous magnesium sulfate,and penetrated with 0.22 μm membrane.The separation of 24 target compounds were performed on an ACQUITY UPLCTM HSS C18 column with gradient elution using acetonitrile-0.1% formic acid/ammonium formate as mobile phase.MS acquisition under positive ion mode was used to obtain accurate relative molecular masses and fragment ions.As a result,the limits of detection(LOD,S/N=3) of the target compounds were in the range of 0.43-10.0 ng/mL.The average recoveries of 24 analytes at three spiked concentration levels ranged from 61% to 98% with relative standard deviations of 1.5%-16.9%.This method could be applied in the analysis of 24 pesticides in putrefied blood due to its fastness,simplicity and relatively high sensitivity. |
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