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Determination of Florfenicol Amine in Aquatic Products by Hydrophilic Interaction hromatography-Tandem Mass Spectrometry  

LIU Zhengcai, ZHANG Qiong, YANG Fang, LIN Yonghui, LIU Suzhen, SU Zhijiao   

  1. Fujian Provincial Key Laboratory of Inspection and Quarantine Technology Research,
    Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Online:2015-02-25 Published:2015-02-16

Abstract:

A method for the determination of florfenicol amine (FFA) in aquatic products was developed by hydrophilic
interaction chromatography-tandem mass spectrometry (HILIC-MS-MS). Samples were extracted with alkalinified ethyl
acetate and cleaned up with n-hexane and lipid adsorbent (LAS). An Acquity UPLC BEH HILIC (55 mm × 2.1 mm, i.d.
1.7 μm) colunm was used for the separation by gradient elution program using acetonitrile-5 mmol/L ammonium acetate
containing formic acid (0.2%) as the mobile phase, and an electrospray ion trap mass spectrometer was used in the positive
ion mode. The FFA was quantified by the matrix-matched external standard method. The results showed that the established
method had a good linear correlation (r2 > 0.990) in the range of 0.1–20 μg/L. The average recoveries of FFA at spiked level
of 1.0–50.0 μg/kg were in the range of 70.5%–87.7% with relative standard deviations (RSDs) of 4.8%–11.6%. The limit of
quantization (LOQ) was 1.0 μg/kg. This method proved to be simple, sensitive, accurate, and suitable for the determination
and confirmation of FFA in aquatic products.

Key words: hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS-MS), aquatic products;florfenicol amine, residue determination

CLC Number: