基于一种直接通过型SPE柱快速检测水产饲料中的地西泮

Rapid detection of diazepam in aquatic feed based on a direct-pass-through SPE column

研究旨在建立一种基于直接通过型固相萃取(SPE)柱结合超高效液相色谱串联质谱的快速、准确测定水产饲料中地西泮的方法。样品经过10 mL乙腈-甲酸水提取、异辛烷除脂后,振荡,离心,将上层清液经直接通过型SPE柱净化,0.22μm滤膜过滤,上机测定。结果显示,地西泮在1.0~10.0μg/L线性范围内线性关系良好,线性系数大于0.99,检测限为0.3μg/kg,定量限为1.0μg/kg。地西泮在空白样品加标的低、中、高3个水平添加量下,回收率在82.6%~101.4%,批内相对标准偏差(RSD)为1.8%~6.2%,批间RSD为3.4%~5.7%。研究表明,该方法省时便捷、节约成本、准确性好,能够满足大规模水产饲料样品的测定。

The research aims to establish a rapid and accurate method for the determination of diazepam in aquatic feed,based on direct solid-phase extraction(SPE)column combined with ultra-high-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).After 10 mL of acetonitrile-formic acid water extraction and defatting with isooctane,the sample is shaken,centrifuged,and the upper clear liquid is purified through direct pass-through SPE column,filtered through a 0.22μm membrane,and then subjected to machine analysis.The results show that the linear coefficient is greater than 0.99,with a detection limit of 0.3μg/kg and a quantification limit of 1.0μg/kg.For diazepam added at low,medium,and high levels to blank samples,the recovery rates range from 82.6% to 101.4%.The intra-batch relative standard deviation(RSD)is between 1.8% and 6.2%,and the inter-batch RSD is between 3.4% and 5.7%.The study indicates that this method is time-efficient,cost-effective,and accurate,making it suitable for the determination of diazepam in large-scale aquatic feed samples.