Chinese Journal of Chromatography ›› 2010, Vol. 28 ›› Issue (11): 1056-1060.DOI: 10.3724/SP.J.1123.2010.01056

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Simultaneous analysis of 4 non-steroidal anti-inflammatory drug residues in mutton muscle using high performance liquid chromatography assisted byultrasonic-microwave extraction

KANG Yongfeng*, ZOU Shiwen, DUAN Wuping, LI Yan, SUN Tao   

  1. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China
  • Received:2010-07-14 Revised:2010-09-10 Online:2010-11-28 Published:2010-11-28

Abstract: A method for the simultaneous determination of 4 non-steroidal anti-inflammatory drug (NSAID) residues, including flunixin meglumine, meloxicam, diclofenac sodium and ketoprofen, in mutton muscle was developed using high performance liquid chromatography assisted by ultrasonic-microwave extraction. The NSAIDs were extracted with acidified ethanol and purified by a diatomite column. The subsequent analysis of NSAIDs was achieved on a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with the mobile phase of acetonitrile-0.2% triethylamine (40:60, v/v, pH 3.5 adjusted by phosphoric acid) at a flow rate of 0.8 mL/min at 30 ℃. The detection wavelength was set at 255 nm. The 4 NSAIDs were well separated within 20 min. The correlation coefficients for 4 NSAIDs were from 0.9993 to 0.9998 with the limits of detection (LOD, S/N=3) of 5~10 μg/kg and the limits of quantification (LOQ, S/N=10) of 15~30 μg/kg. The recoveries were in the range of 65.3%~99.6% with the relative standard deviations (RSDs) less than 15%. This method is simple, rapid and highly sensitive, and can meet the requirement for the qualitative and quantitative analysis.

Key words: high performance liquid chromatography (HPLC), mutton muscle, non-steroidal anti-inflammatory drugs, ultrasonic-microwave assistant extraction