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| Pesticide multiresidue analysis of corn flour using online SFE-SFC-MS/MS techniques |
| Received:May 06, 2021 |
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| KeyWord:supercritical fluid extraction;supercritical fluid chromatography;pesticide residue;corn flour |
| Author Name | Affiliation | E-mail | | ZHANG Danyang | Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin 300191, China | | | JIA Hao | College of Resources and Environment, Jilin Agricultural University, Changchun 130000, China | | | SHI Xiaomeng | Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin 300191, China | | | WANG Ce | Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin 300191, China | | | DENG Kai | Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin 300191, China | | | GENG Yue | Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin 300191, China | gengyue@caas.cn | | LIU Xiaowei | Agro-Environmental Protection Institute, Ministry of Agriculture and Rural Affairs, Tianjin 300191, China | xwliu2006@163.com | | WEI Hong | Huabiao (Tianjin)Technology Co. Ltd, Tianjin 300392, China | |
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| Abstract: |
| In this study, to estimate the concentration of pesticide multiresidue in corn flour, an online supercritical fluid extraction method coupled with supercritical fluid chromatography tandem mass spectrometry(SFE-SFC-MS/MS) was established to facilitate the accurate qualitative and quantitative determination of 71 commonly used pesticide and metabolite residues in corn flour. By comparing different SFE extraction conditions and SFC chromatographic separation parameters, the following online SFE-SFC-MS/MS conditions were found to be optimal:the extraction solvent was a super critical CO2:ethanol mixture(91:9, V/V), static/dynamic extraction time was 5 min, dynamic extraction velocity was 5 mL·min-1, weight ratio of anhydrous magnesium sulfate(dispersant) and the sample was 5:1(m/m), SFC modifier was 0.1% formic acid methanol, gradient elution, flow rate was 1.5 mL·min-1, back pressure regulator A(BPRA) pressure was 14.8 MPa, column temperature was 40 oC, and the post-column compensation solvent was 0.1% formic acid methanol with a flow velocity of 0.05 mL·min-1. Good linearity was achieved(R2>0.99) for the 71 targets, with limits of detection and limits of quantification being 0.003~2.770 μg·kg-1 and 0.01~8.41 μg·kg-1, respectively. The recoveries were in the range of 71.2%~124.6% under fortification levels of 1, 10 μg·kg-1, and 100 μg·kg-1, with relative standard deviation ranging from 1.9%~30.5%. The online supercritical fluid extraction method was less solventconsuming, easier to operate, time saving, and environmentally friendly, which can be useful for detecting pesticide residues in corn flour. |
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