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| Determination of Perchlorate in Tea by Ultra-high Performance Liquid Chromatography-High Resolution Mass Spectrometry Coupled with Dispersive Micro Solid-phase Extraction |
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| DOI： |
| KeyWord:perchlorate dispersive micro solid phase extraction high resolution mass spectrometry tea matrix effect |
| Author | Institution |
| WEI Yu,FANG Cong-rong,ZHAO Yun-feng,CHEN Da-wei,LI Jing-guang |
NHC Key Laboratory of Food Safety Risk Assessment/China National Center for Food Safety Risk Assessment,Beijing，China |
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| Abstract: |
| An ultra high performance liquid chromatography-high resolution mass spectrometry(UHPLC-HRMS) was established for the detection of perchlorate in tea based on dispersive micro solid phase extraction(DMSPE).The samples were extracted with acetonitrile,and cleaned up by DMSPE with PSA and PCX as the adsorbents.The chromatographic analysis was performed on a Poroshell 120 PFP column(50 mm×2.1 mm,1.9 μm) with methanol-1.0% acetic acid aqueous solution as the mobile phase by gradient elution,and the internal standard method was used for quantitation.The qualitative screening and quantitative analysis were carried out in negative ion acquisition mode under targeted single ion monitoring(TSIM)/data dependent mass spectrometry(ddMS2) scanning mode.There was a good linear relationship for perchlorate in the concentration range of 0.05-50 μg/L with its correlation coefficient(r2) of 0.999 7,while the limit of detection(LOD) and the limit of quantitation(LOQ) were 0.4 μg/kg and 1.2 μg/kg,respectively.At three spiked levels of 1.2,12 and 120 μg/kg,the average recoveries for perchlorate in tea ranged from 87.4% to 105%,with the intra day relative standard deviations(RSDr) and the inter-day RSD(RSDR) of 0.30%-6.1% and 4.2%-9.2%,respectively.With the characteristics of easy operation,low cost,superior cleanup effect and high sensitivity which could meet the requirements for EU's residue limit,this method is suitable for the detection of perchlorate in tea,and provides a reliable technical means for monitoring and risk assessment of perchlorate in tea in China. |
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