固相萃取-液相色谱串联质谱法同时测定养殖海水中17种喹诺酮类药物
发布时间：2019-08-13 12:39
【摘要】：建立了固相萃取-液相色谱串联质谱法(SPE-LC-MS/MS)同时检测养殖海水中17种喹诺酮类药物残留的分析方法。海水经酸化处理后,采用HLB固相萃取柱富集、净化目标化合物,通过对比水样在不同上样p H、淋洗液与洗脱液等条件下的回收率,以此对前处理方法进行优化。收集到的洗脱液经氮气吹干后用流动相定容至1 ml,待测。色谱流动相A相为0.1%甲酸水溶液,B相为乙腈,所有药物经梯度洗脱进行分离,在LC-MS/MS正离子模式的多反应监测模式下进行定性定量分析。17种化合物可以在10 min中内得到较好的分离,线性范围为1 200 ng/ml,线性相关系数均大于0.999,检出限均在2 10 ng/L范围内,定量限均在5 20 ng/L范围内。以空白海水为基质,在20、100、200 ng/L三个不同添加水平下采用内标法定量的加标回收率均在71.3% 125.0%范围内,相对标准偏差(RSD)为2.44% 12.27%(n=5)。采用该方法对黄海灵山湾近岸4个养殖场进行海水采集并检测,共检测出4种喹诺酮类药物,分别是恩诺沙星、氧氟沙星、诺氟沙星和环丙沙星,其中,恩诺沙星浓度最高。研究表明,该方法快速、可靠,适用于养殖海水中喹诺酮类药物的检测。
[Abstract]:A method for the simultaneous determination of 17 quinolones residues in cultured seawater by solid phase extraction-liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS) was established. After acidizing, the seawater was enriched by HLB solid phase extraction column to purify the target compounds. The recovery rates of water samples under different conditions, such as pH, eluent and eluent, were compared to optimize the pretreatment method. The collected eluent was dried by nitrogen and then the volume was fixed to 1 ml,. The chromatographic mobile phase A is 0.1% formic acid aqueous solution and B phase is acetonitrile. All the drugs are separated by gradient elution. the 17 compounds can be separated qualitatively and quantitatively in the multi-reaction monitoring mode of LC-MS/MS positive ion mode. 17 compounds can be separated in 10 min, the linear correlation coefficient is 1 鈮，
本文编号：2526131
[Abstract]:A method for the simultaneous determination of 17 quinolones residues in cultured seawater by solid phase extraction-liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS) was established. After acidizing, the seawater was enriched by HLB solid phase extraction column to purify the target compounds. The recovery rates of water samples under different conditions, such as pH, eluent and eluent, were compared to optimize the pretreatment method. The collected eluent was dried by nitrogen and then the volume was fixed to 1 ml,. The chromatographic mobile phase A is 0.1% formic acid aqueous solution and B phase is acetonitrile. All the drugs are separated by gradient elution. the 17 compounds can be separated qualitatively and quantitatively in the multi-reaction monitoring mode of LC-MS/MS positive ion mode. 17 compounds can be separated in 10 min, the linear correlation coefficient is 1 鈮，
本文编号：2526131
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