液相色谱-串联质谱法测定不同基质样品中硝基呋喃代谢物残留量  

Determination of nitrofuran metabolite residues in different samples by liquid chromatography tandem mass spectrometry

作　　者：邢海艳 孙丽 吴旭[1] 鲁素雅 XING Haiyan;SUN Li;WU Xu;LU Suya(Huai’an Institute for Food and Drug Control,Huai’an 223005,China)

机构地区：[1]淮安市食品药品检验所,江苏淮安223005

出　　处：《化学分析计量》2024年第7期101-106,共6页Chemical Analysis And Meterage

摘　　要：建立液相色谱-串联质谱法测定鸡蛋、虾、鱼等农产品中硝基呋喃代谢物的残留量。样品中的硝基呋喃残留物经盐酸水解后,以2-硝基苯甲醛衍生,采用乙酸乙酯提取,浓缩,净化后再用C18色谱柱分离,以0.1%甲酸水溶液-乙腈溶液作为流动相梯度洗脱,电喷雾离子源(ESI)下以多反应监测(MRM)正离子模式扫描检测,内标法定量分析。呋喃它酮代谢物、呋喃西林代谢物、呋喃妥因代谢物、呋喃唑酮代谢物的质量浓度在0.5~50 ng/mL范围内与色谱峰面积线性关系良好,相关系数均大于0.995,检出限分别为0.13、0.035、0.14、0.017μg/kg。在鸡蛋、虾、鱼中添加2、5、10μg/kg硝基呋喃代谢物时,平均回收率为88.71%~105.16%,测定结果的相对标准偏差为3.12%~9.08%(n=6)。该方法简便、快捷、准确度高,可用于测定鸡蛋、虾、鱼等农副产品中的硝基呋喃代谢物。A liquid chromatography-tandem mass spectrometry method was established for the determination of nitrofuran metabolites residues in eggs,shrimp,fish and other agricultural products.The nitrofuran residue in the sample was hydrolyzed by hydrochloric acid,derived with 2-nitrobenzaldehyde,extracted with ethyl acetate,concentrated and purified,and then separated by C18 chromatographic column,with 0.1%formic acid aqueous solution-acetonitrile solution as mobile phase gradient elution,electrospray ion source(ESI)under multiple reaction monitoring(MRM)positive ion mode scanning detection,quantitative analysis by internal standard method.The mass concentration of furaltadone metabolite,nitrofurazone metabolite,nitrofurantoin metabolite and furazolidone metabolite had a good linear relationship with the chromatographic peak area in the range of 0.5-50 ng/mL,and the correlation coefficients were all greater than 0.995.The detection limits were 0.13,0.035,0.14 and 0.017μg/kg,respectively.When 2,5 and 10μg/kg nitrofuran metabolites were added to eggs,shrimp and fish,the average recoveries were 88.71%-105.16%,and the relative standard deviations of the determination results were 3.12%-9.08%(n=6).The method is simple,rapid and accurate,and can be used for the determination of nitrofuran metabolites in eggs,shrimp,fish and other agricultural by products.

关 键 词：硝基呋喃代谢物 液相色谱-串联质谱法 衍生化 鸡蛋 鱼 虾 

分 类 号：O657.7[理学—分析化学]