液相色谱串联质谱法测定大菱鲆和鳜鱼体中地西泮及其代谢物残留的研究

Determination of diazepam and its residue in turbot and mandarinfish by high performance liquid chromatography-tandem mass spectrometry

建立了高效液相色谱-串联质谱(HPLC/MS/MS)测定鱼类样品中地西泮及其代谢物去甲地西泮、替马西泮和奥沙西泮的分析方法。样品用1%氨化乙酸乙酯提取,HLB固相萃取柱净化,乙酸乙酯洗脱。在正离子模式下以电喷雾串联质谱仪进行测定,以氘代地西泮、氘代去甲地西泮、氘代替马西泮和氘代奥沙西泮为内标物,内标法定量。以大菱鲆和鳜鱼为研究对象,在1.0、10.0和50.0μg/kg添加水平下,方法平均回收率为85.7%～105.6%(批内),相对标准偏差为2.1%～7.6%(批内),方法定量限为1.0μg/kg(S/N>10)。实验结果表明:该方法简单、快速、准确度高、重复性好,适合于鱼类样品中地西泮及其代谢物残留的检测。

A method for detecting residues of diazepam, nordiazepam, temazepam and oxazepam in aquatic products was developed by using high performance liquid chromatography-tandem mass spectrometry （HPLC/MS/MS）. Dia- zepam and its metabolites was extracted with basic ethyl acetate from the test tissue, then the extract was cleaned up and concentrated on an Oasis HLB cartridge, eluted by ethyl acetate and then analyzed by HPLC - MS/MS. The quantification was performed with internal standard method, the D5 -diazepam, D5 - nordiazepam, D5 -temazepam and D5 -oxazepam were taken as internal standard. The average recoveries were 85.7% -105.6% （intraday） , the relative standard deviations were 2.1% -7.6 % （intraday） in the spiked range of 1.0,10.0 and 50 μg/kg. The limits of quantification （S/N 〉 10） were 1.0μg/kg . The results indicated that the method developed is easy, fast, and accurate and is applicable to be used for detection of diazepam and its metabolic residues.