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

作　　者：谢云峰 李少晖 任丹丹 刘佳 安学静[2] 杨永坛 

机构地区：[1]中粮营养健康研究院营养健康与食品安全北京市重点实验室,北京102209 [2]北京工业大学生命科学与生物工程学院,北京100022

出　　处：《分析测试技术与仪器》2015年第4期212-217,共6页Analysis and Testing Technology and Instruments

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％～15．6％之间。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 - 50 μg/kg and all the R2 were greater than 0. 995. The LODs for the metabolites were 0.2 μg/kg and the LOQs were 0.5 μg/kg. The average recoveries for the blank pork samples at three spiked levels （0.5,1.0 and 10.0 μg/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.

关 键 词：硝基呋喃 代谢物 超高效液相色谱-串联质谱法 猪肉 

分 类 号：O657.7[理学—分析化学]