超高效液相色谱串联质谱法对水产品中硝基呋喃代谢物的测定

建立了使用Waters UPLC Xevo TQ超高效液相色谱串联质谱仪检测水产品中4种硝基呋喃代谢物的分析方法。匀浆后的样品在酸性环境下水解,并用2-硝基苯甲醛衍生16h,经磷酸氢二钾提取,LMS固相萃取小柱净化后,在三重四极杆多反应监测模式下进行测定。方法采用同位素内标法定量,四种代谢物的检出限(LOD)均低于0.25μg·kg-1,线性范围在0.5μg·L~(-1)到10μg·L~(-1)间,相关系数大于0.99。在0.5、1.0和5μg·kg-1浓度下分别进行添加回收试验(n=5),回收率在75.2%~123.3%之间,相对标准偏差(RSD)小于9.4%。

Determination of nitrofuran metabolites in aquatic products by ultra performance liquid chromatography tandem mass spectrometry

The analysis method was established using the waters UPLC Xevo TQ ultra performance liq‐uid chromatography -tandem mass spectrometry to detect 4 nitrofuran metabolites in aquatic prod‐ucts .After hydrolyzed in acidic environment ,and derivated by 2 -nitrobenzaldehyde for 16h ,then extracted by dipotassium hydrogen phosphate ,and purified by LMS solid phase extraction column ,ho‐mogenate samples were measured in triple quadruple multiple reaction monitoring mode .The quanti‐ties of the metabolites was determined by isotope internal standard method ,which detection limit (LOD) were up to 0 .25 μg · kg -1 ,the linear range of the method was 0 .5~10 μg · L -1 ,and the cor‐relation coefficient was more than 0 .99 .Recovery tests were carried out under the concentration of 0.5 ,1 and 5 μg · L -1 respectively ,the recovery rate was 81 .2% ~113 .7% ,with the relative standard deviation (RSD) less than 9 .4% .