Citation: LI Jiong, ZHENG Xin, WANG Hongqing, QIU Hongyu. Determination of fipronil and its metabolites in bird eggs by ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction[J]. Chinese Journal of Chromatography, ;2017, 35(12): 1211-1215. doi: 10.3724/SP.J.1123.2017.08018 shu

Determination of fipronil and its metabolites in bird eggs by ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction

1.
Hangzhou Institute for Food and Drug Control, Hangzhou 310017, China;
2.
Shimadzu(China) Co., Ltd. Beijing Branch, Beijing 100020, China

Received Date: 25 August 2017

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed to determine fipronil and its metabolites (fipronil desulfinyl, fipronil sulfone and fipronil sulfide) in bird eggs. The samples were extracted with acetonitrile containing 0.1%(v/v) acetic acid, and then purified by a mixture of anhydrous sodium sulfate, octadecyl carbon silica gel (C₁₈-N) sorbent and ethylenediamine-N-propyl carbon silica gel (NH₂-PSA) sorbent. The analysis was performed by a UPLC-MS/MS system with Shim-pack GIST C₁₈ column (50 mm×2.1 mm, 2 μm). The mobile phases consisted of methanol and 1 mmol/L ammonium acetate aqueous solution by gradient elution, and multiple reaction monitoring (MRM) mode with negative electrospray ionization was used. The effect of the dosages of anhydrous sodium sulfate, C₁₈-N and NH₂-PSA in cleaning-up agent was studied. The main influence factors and analytical conditions were modified. Four linear calibration curves were obtained with correlation coefficients r² ≥ 0.9989. The recoveries were determined at three concentrations and ranged from 95.09%-103.26%. The limit of quantification (LOQ) was 0.2 μg/kg. It is suitable for the determination of fipronil and its metabolites in bird eggs.
- ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- dispersive solid phase extraction,
- fipronil,
- bird eggs
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1.
沈阳化工大学材料科学与工程学院沈阳 110142