Kang Yongfeng, Zou Shiwen, Duan Wuping, Li Yan, Sun Tao
College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China.
Se Pu. 2010 Nov;28(11):1056-60.
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 x 4.6 mm, 5 microm) 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 degrees C. 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 0.999 3 to 0.999 8 with the limits of detection (LOD, S/N = 3) of 5-10 microg/kg and the limits of quantification (LOQ, S/N = 10) of 15-30 microg/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.
建立了一种利用超声-微波辅助萃取的高效液相色谱法同时测定羊肉肌肉中4种非甾体抗炎药(NSAID)残留量的方法,这4种药物包括氟尼辛葡甲胺、美洛昔康、双氯芬酸钠和酮洛芬。NSAID用酸化乙醇萃取,并用硅藻土柱净化。随后在Hypersil C18柱(250 mm×4.6 mm,5μm)上进行NSAID分析,流动相为乙腈-0.2%三乙胺(40∶60,v/v,用磷酸调节pH至3.5),流速为0.8 mL/min,柱温30℃。检测波长设定为255 nm。4种NSAID在20 min内得到良好分离。4种NSAID的相关系数在0.999 3至0.999 8之间,检测限(LOD,S/N = 3)为5 - 10μg/kg,定量限(LOQ,S/N = 10)为15 - 30μg/kg。回收率在65.3% - 99.6%范围内,相对标准偏差(RSD)小于15%。该方法简便、快速且灵敏度高,能够满足定性和定量分析的要求。