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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0.5～10μg/kg,DN-SH的线性相关系数为0.999 5,检出限为0.5μg/kg。在0.5、1.0、2.0和4.0μg/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。
To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of DNSH residues in Nifuzuol metabolites in animal-derived foods. The sample was hydrolyzed with hydrochloric acid and derivatized with 2-nitrobenzaldehyde. The sample was purified and identified by liquid chromatography-electrospray triple quadrupole tandem mass spectrometry (MS-MS / MS). Multiple reaction monitoring (MRM) was used to optimize mass spectrometry parameters and quantification by internal standard method. The linear range of this method was 0.5 ~ 10μg / kg, the linear correlation coefficient of DN-SH was 0.999 5, the detection limit was 0.5μg / kg. The spiked recoveries ranged from 63.4% to 109.5% with RSD ranging from 2.0% to 11.9% at the concentration of 0.5, 1.0, 2.0 and 4.0 μg / kg. The method has high sensitivity, good reproducibility and is suitable for confirming and confirming the residual amount of 3,5-dinitrosalicylic hydrazine in Nifursellol metabolites in animal-derived foods.