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| Determination of Neonicotinoid Residues in Honey by Target Single Ion Monitoring/High Resolution Mass Spectrometry Combined with Salting-out Assisted Liquid-Liquid Extraction and PVPP Cleanup |
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| DOI： |
| KeyWord:neonicotinoid pesticides polyvinylpolypyrrolidone(PVPP) target single ion monitoring (TSIM) high resolution mass spectrometry honey salting out assisted liquid liquid extraction |
| Author | Institution |
| L? Bing,XIN Shao-kun,CHEN Da-wei,ZHAO Yun-feng |
国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室 |
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| Abstract: |
| Based on salting-out assisted liquid-liquid extraction(LLE) and polyvinylpolypyrrolidone(PVPP) cleanup,a method was developed for the determination of seven neonicotinoid pesticides in honey by target single ion monitoring(TSIM)/high-resolution mass spectrometry.The samples were extracted and cleaned up with acetonitrile by salting-out assisted LLE-PVPP method.The chromatographic separation was conducted on a BEH C18 column using methanol-water containing 0.1%formic acid and 5 mmol/L ammonium formate in two phases,as mobile phase by gradient elution.The analysis was performed by high resolution mass spectrometry in TSIM mode,and the quantitation was carried out by the internal standard method.The result showed that salting-out assisted LLE-PPVP cleanup method allowed one-step sample preparation,while TSIM mode showed a wide linear dynamic range with higher sensitivity and accuracy.There existed good linearities(r2>0.999) for seven neonicotinoid pesticides in the concentration ranges of 0.01-100 μg/L or 0.02-100 μg/L.The limits of detection(LODs) and quantitation(LOQs) were in the ranges of 0.03-0.07 μg/kg and 0.1-0.2 μg/kg,respectively.At three spiked levels of 0.2,2,20 μg/kg,the average recoveries for the analytes in honey were between 84.8%and 112.7%,with the intra-day precision(RSDr) and the inter-day precision(RSDR) of 0.9%-5.7%and 3.7%-9.7%,respectively.With the advantages of a rapid and simple pretreatment,low-cost,high sensitivity and good reproducibility,this method was suitable for the determination of neonicotinoid pesticides in honey. |
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