分散固相萃取-高效液相色谱串联质谱法同时测定沉积物中氟喹诺酮类药物残留  

Simultaneous determination of fluoroquinolones residues in sediment by dispersive solid-phase extraction combined with high performance liquid chromatography-tandem mass spectrometry

作　　者：钱卓真[1] 梁焱 王丽娟[1] 汤水粉[1] 罗方方[1] 陈思 QIAN Zhuozhen;LIANG Yan;WANG Lijuan;TANG Shuifen;LUO Fangfang;CHEN Si(Key Laboratory of Cultivation and High-value Utilization of Marine Organisms in Fujian Province,Fisheries Research Institute of Fujian,Xiamen 361013,China;Hainan Province Environmental Monitoring Centre,Haikou 570026,China)

机构地区：[1]福建省水产研究所福建省海洋生物增养殖与高值化利用重点实验室,福建厦门361013 [2]海南省环境科学研究院,海南海口570026

出　　处：《渔业研究》2018年第4期286-294,共9页Journal of Fisheries Research

基　　金：福建省省属公益类科研院所基本科研专项(2015R1003-7);福建省自然科学基金面上项目(2018J01056)

摘　　要：本文建立了分散固相萃取结合高效液相色谱-串联质谱同时测定沉积物中氟喹诺酮类药物残留的分析方法。沉积物经20 m L乙腈-磷酸盐(1∶1,V/V)缓冲液超声提取,0.15 g乙二胺四乙酸二钠络合除杂,分散固相萃取材料净化,Ultimate XB-C18色谱柱分离,含4 mmol/L乙酸铵的0.1%甲酸水溶液-0.1%甲酸甲醇梯度洗脱,电喷雾正离子模式下以多反应监测方式检测,内标法定量分析。通过试验优化了不同提取方法、净化吸附剂比。结果表明,5种氟喹诺酮类药物在2.5~200 ng/m L范围内线性关系良好(R2>0.99),方法定量限(S/N≥10)为2μg/kg。在2~50μg/kg添加水平内,平均回收率为79.8%~112%,日内相对标准偏差(RSD)为3.2%~9.9%,日间RSD为5.3%~8.6%。An efficient method was established for the determination of fluoroquinolones in sediment by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） combined with dispersive solid-phase extraction. The samples were ultrasonically extracted with 20 m L phosphate buffer solution and acetonitrile mixture（1∶ 1,V/V）,followed by 0. 15 g ethylenediamine tetraacetic acid disodium salt complexation. Then the supernatant extract was cleaned up with a dispersive solid-phase extraction. The analytes were separated on a Ultimate XB-C18 column by gradient elution with 4 mmol/L ammonium acetate-0. 1%formic acid-0. 1% formic acid methol as mobile phase,detected in multiple reaction monitoring（MRM）with electrospray ionization（ESI） under positive ion mode. And the quantitative results were calculated by the internal standard method. The results showed that the calibration curves were linear（R2 0. 99） in the range of 2. 5 - 200 ng/m L for five fluoroquinolones. Limits of quantitation for fluoroquinolones were 2 μg/kg.The average recoveries at spiked levels of 2 - 50 μg/kg ranged from 79. 8% to 112%. Intra-day and inter-day RSDs were 3. 2% - 9. 9% and 5. 3% - 8. 6%,respectively.

关 键 词：沉积物 氟喹诺酮 分散固相萃取 高效液相色谱串联质谱法 

分 类 号：X833[环境科学与工程—环境工程]