Yang Wanghuo, Wu Shaoming, Cai Xiaoming, Feng Lifeng, Chen Yankai, Li Yanping, Liang Min
National Quality Supervision and Testing Center for Processed Food, Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China.
Se Pu. 2017 Oct 8;35(10):1062-1067. doi: 10.3724/SP.J.1123.2017.06029.
A method for the determination of 29 imidazoles and their metabolites in pork by liquid chromatography-tandem mass spectrometry has been developed. The samples were extracted with ethyl acetate, and then defatted with -hexane after concentration of the extracts. The analytes were separated on a C reversed-phase column with 0.3% (v/v) formic acid aqueous solution and acetonitrile as mobile phases, and finally analyzed using electrospray ionization in positive ion mode (ESI) with multiple reaction monitoring (MRM). The linear ranges of the 29 compounds were from 0.05 to 20.0 μg/L with the correlation coefficients () more than 0.99. The average recoveries and relative standard deviations were 65.4%-103% and 1.3%-6.8% respectively in the spiked ranges of 1.0-5.0 μg/kg. The limits of detection and the limits of quantification were 0.02-0.3 μg/kg and 0.1-1 μg/kg respectively for the 29 imidazoles. The method is simple, rapid and sensitive. It is suitable for the detection of imidazoles and their metabolites in pork.
建立了一种液相色谱-串联质谱法测定猪肉中29种咪唑及其代谢物的方法。样品用乙酸乙酯萃取，萃取液浓缩后用正己烷脱脂。分析物在C反相柱上分离，以0.3%（v/v）甲酸水溶液和乙腈为流动相，最后采用电喷雾电离正离子模式（ESI）和多反应监测（MRM）进行分析。29种化合物的线性范围为0.05至20.0μg/L，相关系数（）大于0.99。在1.0-5.0μg/kg的加标范围内，平均回收率和相对标准偏差分别为65.4%-103%和1.3%-6.8%。29种咪唑的检测限和定量限分别为0.02-0.3μg/kg和0.1-1μg/kg。该方法简便、快速、灵敏，适用于猪肉中咪唑及其代谢物的检测。
