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目的建立一种采用液相色谱-串联质谱法检测水产品中硝呋索尔代谢物残留量的测定方法。方法样品中以结合态形式残留的硝呋索尔代谢物3,5-二硝基水杨酸肼(DNSAH)经盐酸水解,2-硝基苯甲醛衍生,用乙腈提取,以电喷雾离子源负离子扫描模式进行质谱分析,内标法定量。结果 DNSAH在0.2~20μg/L范围内线性关系良好,相关系数r~2>0.999。DNSAH添加水平为0.50~5.00μg/kg时,平均回收率在88.3%~100%之间,批内和批间变异系数均<15%。DNSAH的检出限为0.20μg/kg。结论本方法灵敏、高效、简单、重现性好,满足水产品中硝呋索尔代谢物残留量的检测。
Objective To establish a method for the determination of residual Nifuzuol metabolites in aquatic products by liquid chromatography-tandem mass spectrometry. Methods Residual nitrofurant metabolites 3,5-dinitrosalicylic hydrazide (DNSAH), which were bound in the bound form, were hydrolyzed by hydrochloric acid, derivatized with 2-nitrobenzaldehyde and extracted with acetonitrile. Electrospray ionization Negative ion scan mode for mass spectrometry, internal standard method. Results DNSAH had a good linearity in the range of 0.2 ~ 20μg / L with a correlation coefficient of r ~ 2> 0.999. When the DNSAH level was 0.50 ~ 5.00μg / kg, the average recoveries ranged from 88.3% to 100%, and the variation coefficients within and between batches were all <15%. The detection limit of DNSAH was 0.20 μg / kg. Conclusion The method is sensitive, efficient, simple and reproducible. It can meet the requirement of Nifursellol metabolite residues in aquatic products.