Determination of Pendimethalin Residues in Aquatic Products from Rice Fields by QuEChERS-high Performance Liquid Chromatography-tandem Mass Spectrometry
Determination of Pendimethalin Residues in Aquatic Products from Rice Fields by QuEChERS-high Performance Liquid Chromatography-tandem Mass Spectrometry
A method based on Quick,Easy,Cheap,Effective,Rugged and Safe(QuEChERS)dispersive solid-phase extraction coupled with high performance liquid chromatography tandem mass spectrometry was developed for the determination of pendimethalin in aquatic products.The samples were extracted with ethyl acetate containing 0.1%(V/V)formic acid,and the extracts were purified by dispersive solid-phase extraction with 0.6 g polystyrene-divinylbenzene(PS-DVB)and 0.2 g primary secondary amine(PSA)sorbents.The purified extracts were collected and concentrated at 40℃to almost dry under nitrogen gas.The resulting extracts were re-dissolved in 1.0 mL of acetonitrile,filtered through microfiltration membrane(0.22 μm),and analyzed by high performance liquid chromatography-tandem mass spectrometry.The target compounds were separated on a Kinetex C18 column(100 mm×2.1 mm,2.6 μm),and gradient elution was performed with acetonitrile and 0.1%(V/V)aqueous formic acid solution.Electrospray ion source(ESI)and selective reaction monitoring(SRM)were used for analysis,and the matrix-matched internal standard method was used for qualitative and quantitative determinations.The results showed that good linear relationship was in the range of 2～100 μg/L,with the correlation coefficient being 0.999 5.The limits of detection(LOD)and quantitation(LOQ)were 0.5 μg/kg and 1.0 μg/kg,respectively.The average recoveries of pendimethalin at three different spiking levels in a sample matrix carp,procambarus clarkiir or pelodiscus sinensis ranged from 78.9%to 110.6%,with RSDs ranging from 3.8%to 6.8%under.This method has the advantages of high speed,accuracy and sensitivity,and can meet the requirements for detecting pendimethalin residue in aquatic products from rice fields.
关键词
高效液相色谱-串联质谱法/QuEChERS法/二甲戊灵/稻田水产品
Key words
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/QuEChERS/pendimethalin/paddy field aquatic products
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