Citation: LIU Yongqiang, LIU Sheng, XU Wenjuan, TIAN Guoning, ZHANG Jinling. Rapid screening of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry[J]. Chinese Journal of Chromatography, ;2017, 35(9): 941-948. doi: 10.3724/SP.J.1123.2017.06001 shu

Rapid screening of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

1.
Technical Center for Inspection & Quarantine of Weifang Entry-Exit Inspection & Quarantine Bureau, Weifang 261041, China;
2.
Technical Center for Inspection & Quarantine of Zibo Entry-Exit Inspection & Quarantine Bureau, Zibo 255035, China

Received Date: 31 May 2017

Fund Project: Program of Shandong Entry-Exit Inspection & Quarantine Bureau (No. SK201613)

An analytical method was established for the simultaneous determination of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS). The samples were extracted with acetonitrile containing 0.1% (v/v) acetic acid aqueous solution, and cleaned-up by primary secondary amine (PSA) and octadecyl bonded silica (C₁₈) adsorbents. The compounds were separated on a Poroshell 120 SB-C₁₈ column (100 mm×3.0 mm, 2.7 μm) with 0.1% (v/v) formic acid aqueous solution containing 5 mmol/L ammonium acetate-acetonitrile as mobile phases under gradient elution. The eluent was determined by UPLC-Q-TOF/MS with electrospray ionization in positive mode. The quantification analysis was performed with the external standard method. In all ions MS/MS mode, the compounds were qualitatively screened and confirmed by one data acquisition. The correlation coefficients (r) were greater than 0.995 in the linear ranges of the 44 pesticides. The limits of quantification (LOQs, S/N=10) of the 44 pesticides were 2.5-5.0 μg/kg. At the three spiked levels, the recoveries were between 73.4% and 113.7% with the relative standard deviations (RSDs) ranging from 0.7% to 12.1% (n=6). The method effectively improves the determination efficiency of pesticide residues screening by high-resolution mass spectrometry.
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沈阳化工大学材料科学与工程学院沈阳 110142