高效液相色谱-串联质谱法检测动物源食品中硝呋索尔代谢物残留

建立动物源食品中硝呋索尔代谢物3,5-二硝基水杨酸肼（DNSH）残留量的液相色谱 串联质谱（LC-MS/MS）检测方法。样品经盐酸水解，2-硝基苯甲醛衍生，提取净化后，用液相色谱 电喷雾三重四极杆串联质谱检测，多反应监测模式（MRM）优化质谱参数，内标法定量。该方法的线性范围为0.5~10 μg/kg，DNSH的线性相关系数为0.999 5，检出限为0.5 μg/kg。在0.5、1.0、2.0和4.0 μg/kg的浓度添加水平下，加标回收率为63.4%~109.5%，RSD为2.0%~11.9%。本方法灵敏度高、重现性好，适用于动物源食品中硝呋索尔代谢物3,5-二硝基水杨酸肼残留量的确证检测。

Determination of the Metabolite of Nifursol in Animal Origin Food by HPLC-MS/MS

A method of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the determination of 3,5-dinitrosalicylic acid hydrazine (DNSH)，which was the metabolite of nifursol antibiotic in animal origin food. The samples were hydrolyzed with 0.1 mol/L HCl, and derivatised with 2-nitrobenzaldehyde at 37 ℃ for 16 h. The derivative solutions were adjusted to pH 7.0-7.5, and extracted by ethyl acetate. The analyte was detected by tandem mass spectrometry with electrospray ionization source by MRM mode. There is good linear correlation between the peak areas and concentrations of DNSH(the calibration coefficient is 0.999 5), the dynamic linear range is 0.5-10 μg/kg. The limit of detection (S/N=3) is 0.5 μg/kg. The recoveries of DNSH at four spiked levels of 0.5, 1.0, 2.0, 4.0 μg/kg range from 63.4% to 109.5% (n=6) and the RSDs are between 2.0% and 11.9% (n=6). It is proved to be fast and effective for simultaneously qualitative and quantitative inspection of the metabolite of nifursol antibiotic in animal origin food.