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| Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction |
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| DOI： |
| KeyWord:pesticide residues cold induced liquid－liquid extraction high resolution mass spectrometry vegetables fruits QuEChERS |
| Author | Institution |
| BI Jun，REN Jun，ZHAO Yun-feng，CHEN Da-wei |
1. NHC Key Laboratory of Food Safety Risk Assessment， China National Center for Food Safety Risk Assessment， Beijing ， China;2. Panjin Center for Inspection and Testing， Panjin ， China;3. Wuhai Inspection and Testing Center， Wuhai ， China |
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| Abstract: |
| Based on QuEChERS and cold induced liquid－liquid extraction（CI－LLE） technique， an analytical method for the determination of 77 pesticide residues in vegetables and fruits was developed by ultra-high performance liquid chromatography－high resolution mass spectrometry. The samples were extracted， salted out， and cleaned up by traditional QuEChERS method， and further enriched and cleaned up by CI－LLE technique using 40% acetonitrile－water solution. The chromatographic separation of pesticides was performed on a C18 column（2.1 mm × 150 mm， 2.6 μm） using water－methanol （containing 0.1% formic acid and 4 mmol/L ammonium formate for each） as mobile phases by gradient elution. The pesticides were analyzed by the high resolution mass spectrometry in full scan mode by time sediment， and quantified by internal standard method. Results showed that 77 pesticides had good linearity in the certain concentration ranges with relative coefficients（r2） larger than 0.99. The limits of detection and limits of quantitation were in the ranges of 0.02－0.20 μg/kg and 0.05－0.50 μg/kg， respectively. At four different spiked levels， the recoveries for pesticides in vegetables and fruits ranged from 70.8% to 119%， with relative standard deviations（RSDs） of 0.70%－15%. The method is simple and reproducible， and could be used to reduce matrix effect on the detection of pesticide residues with high sensitivity， accuracy， and precision. Therefore， it could meet the requirements for multi-residue detection of pesticides， and be applied to the qualitative and quantitative determination of pesticides in real samples. |
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