超高效液相色谱-串联质谱法测定猪肉中硝基呋喃类代谢物

Determination of Nitrofuran Metabolites in Pork by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定猪肉组织中4种硝基呋喃类代谢物的分析方法.样品经盐酸水解,2-硝基苯甲醛衍生,乙酸乙酯提取净化,在正离子模式下以电喷雾电离串联质谱进行测定,内标法定量.在优化的实验条件下,4种代谢物在0.5~50μg/kg范围内线性良好,相关系数大于0.995,方法检出限为0.2μg/kg,定量限为0.5μg/kg.在0. 5、1.0和10.0μg/kg的添加水平下,4种代谢物的平均回收率在74.6%~104.8%之间,相对标准偏差(RSD, n=6)在2.4%~

     

    Abstract: An analytical method for the determination of 4 nitrofuran metabolites in pork has been developed based on the ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The metabolites in pork samples were hydrolized in hydrochloric acid, and derivatized with 2-nitrobenzaldehyde. After the extraction and concentration with ethyl acetate, the analytes were determined by UPLC-MS/MS in the multiple reaction monitoring mode using an internal standard method. Under the optimized conditions,all the analytes were in good linearity at the range of 0.5~50μg/kg and all the R2 were greater than 0.995. The LODs for the metabolites were 0.2μg/kg and the LOQs were 0.5μg/kg.The average recoveries for the blank pork samples at three spiked levels(0.5,1.0 and 10.0μg/kg) ranged from 74.6% to 104.8%,with the relative standard deviations(RSDs, n=6) of 2.4%~15.6%.The proposed method is rapid, accurate and sensitive, and is suitable for the detection of nitrofuran metabolites in pork.

     

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