摘要
优化了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定养殖水质中地西泮的分析方法。水样经双层定性滤纸过滤,通过HLB柱富集净化,用乙腈洗脱后吹干,50%甲醇水溶液溶解残渣。后经ZORBAX Eclipse Plus C18(50.0 mm×2.1 mm,1.8μm)色谱柱分离,0.2%甲酸甲醇溶液和0.2%甲酸乙酸铵水溶液为流动相进行梯度洗脱。采用电喷雾正离子电离,多反应监测(MRM)模式下测定,内标法定量。地西泮在20.0~2000.0 ng/L内的线性关系良好,相关系数(r^(2))>0.9996。方法检出限、定量限分别为10.0和20.0 ng/L。平均加标回收率为92.6%~101.7%,相对标准偏差(RSD)(n=6)为4.68%~5.97%。指出,该方法提高了检测效率,降低检测成本,可满足养殖环境中大批量水质样品中地西泮的测定需求。
To optimize the analytical method for determination of diazepam in aquaculture water samples based on ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),water samples were filtered through double qualitative filter paper,and subsequently enriched with a hydrophile lipophile balance solid phase extraction(HLB SPE)cartridge.The purified extracts were eluted with acetonitrile,and then dried.The dried residues were redissolved with 1 mL 50%methanol water solution for UPLC-MS/MS analysis.The chromatographic separation of diazepam were performed on a ZORBAX Eclipse Plus C18(50.0 mm×2.1 mm,1.8μm)column by gradient elution,with 0.2%formic acid methanol solution and 0.2%formic acid amine acetate solution as mobile phases.Diazepam was determined with positive electrospray ionization under multiple reaction monitoring(MRM)mode,and quantified by internal standard method.Good linear relationships for diazepam was obtained in the range of 20.0-2000.0 ng/L with correlation coefficients(r^(2))larger than 0.9996.The detection limit of the method for aquaculture water samples was 10.0 ng/L,while the quantitation limit was 20.0 ng/L,respectively.The average recoveries for spiked negative aquaculture water ranged from 92.6%to 101.7%,with relative standard deviations(RSDs,n=6)between 4.68%and 5.97%.The proposed method is rapid and accurate,and it is suitable for the residual determination of diazepam in real aquaculture water samples.
作者
张静波
王雨琪
徐汇宏
陆悦
朱正华
黄强
ZHANG Jingbo;WANG Yuqi;XU Huihong;LU Yue;ZHU Zhenghua;HUANG Qiang(Aquatic Products Quality Testing Center of Nantong,Nantong,Jiangsu 226000,China)
出处
《水产养殖》
CAS
2024年第8期7-11,共5页
Journal of Aquaculture
基金
2022年度南通市民生科技计划项目(MS22022076)。
