摘要
建立一种快速测定水产中地西泮的方法。5%氨水乙腈提取,通过EMR固相萃取柱净化,旋蒸浓缩并定容,用内标法对其进行定量。通过超高效液相色谱串联质谱仪测定,使用Agilent ZORBAX Eclipse Plus RRHD C 18柱子分离,流动相乙腈:0.1%甲酸水,内标法定量,该方法测得的地西泮检出限0.33μg·kg^(-1)和定量限1.1μg·kg^(-1),对样品进行1.10,3.30,11.0μg·kg^(-1)三个梯度加标,平均回收率85.6%~103.3%,精密度为0.8%~3.5%。该研究方法提取简单,回收率和精密度满足要求,可为水产中地西泮残留的检测标准制定提供依据。
To establish a method for rapid determination of diazepam in aquatic products was developed.5%acetonitrile was extracted from ammonia,purified by EMR solid phase extraction column,condensed by rotary distillation and fixed volume,quantified by internal standard method.Determined by ultra-high performance liquid chromatography tandem mass spectrometer,separated by Agilent ZORBAX Eclipse Plus RRHD C 18 column,mobile phase acetonitrile:0.1%formic acid water was quantified by internal standard method.The detection limit of diazepam measured by this method was 0.33μg·kg^(-1)and the quantification limit was 1.1μg·kg^(-1).The samples were subjected to three gradient labeling methods:1.10,3.30 and 11.0μg·kg^(-1).The average recovery was 85.6%~103.3%,and the precision was 0.8%~3.5%.The method is simple to extract,the recovery rate and precision meet the requirements,and can provide a basis for the determination of diazepam residues in aquatic products.
作者
王若男
徐朝华
胡飞燕
Wang Ruonan;Xu Zhaohua;Hu Feiyan(Jiangmen Polytechnic,Jiangmen 529090,China)
出处
《山东化工》
2023年第24期124-126,129,共4页
Shandong Chemical Industry
关键词
苯二氮卓类
地西泮
水产品
前处理
高效液相串联质谱
benzodiazepines
diazepam
aquatic products
pre-treatment
ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry
