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Citation: ZHOU Peng, HUANG Qian, OUYANG Liqun, WANG Zheng, MENG Peng, DAI Ming, WANG Ying. Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2018, 36(7): 629-633. doi: 10.3724/SP.J.1123.2018.01049 shu

Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry

ZHOU Peng ^1,2, ,
HUANG Qian ² ,
OUYANG Liqun ² ,
WANG Zheng ² ,
MENG Peng ² ,
DAI Ming ² ,
WANG Ying ¹

1.
School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China;
2.
National Center for Quality Supervision Inspection of Processed Foods(Fuzhou), Fuzhou 350002, China

Received Date: 30 January 2018

A method based on ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established for the determination of fipronil and its metabolites in feeds. Sodium chloride was added to the samples after the ultrasonic extraction of pure water and acetonitrile, and then cleaned up by the QuEChERS method. The target analytes were separated on a Waters HSS T3 C₁₈ column using methanol and water as mobile phases with gradient elution, and detected by a MS/MS system under negative electro-spry ionization (ESI^-) and the multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 0.05 μg/kg, and the limits of quantification (LOQs) were 0.2 μg/kg. The linear correlation coefficients were more than 0.9998. The average recoveries ranged from 92.3% to 105.4% with RSDs no more than 2.3%. This method is suitable for the identification of fipronil and its metabolites in feeds because of its simplicity and high sensitivity.
- ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS),
- QuEChERS,
- isotope dilution,
- fipronil and its metabolites,
- feeds
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