SPE-HPLC-MS/MS检测地表水中的萘啶酸、吡哌酸、培氟沙星、氧氟沙星、司帕沙星和加替沙星残留

Determination of nalidixic acid,pipemidic acid,pefloxacin,ofloxacin,sparfloxacin and gatifloxacin residues in surface water by SPE-HPLC-MS/MS

该实验建立全自动固相萃取-HPLC-MS/MS法检测地表水中的萘啶酸、吡哌酸、培氟沙星、氧氟沙星、司帕沙星和加替沙星残留的分析方法。随机采集地表水样并过滤,将pH调节至中性。将预处理好的地表水样品,以流量为8~10 mL/min的速度过已活化的固相萃取柱,再用10 mL 5%甲醇溶液淋洗、净化,弃去淋洗液,抽干小柱,最后用20 mL甲醇洗脱,收集洗脱液;洗脱液氮吹至近干,用乙腈定容至1 mL,涡旋混合1 min,上HPLC-MS/MS仪定量检测。结果表明吡哌酸、氧氟沙星、培氟沙星、司帕沙星、加替沙星和萘啶酸在质量浓度0.01~8.00μg/mL范围内线性关系良好,相关系数均大于0.995;检出限分别为1.82,1.39,2.41,1.49,1.93,1.12μg/L;方法加标回收率在84.2%~92.2%之间;重复性相对标准偏差(n=6)在5.0%以内。此方法具有处理速度快、检测结果可靠等特点,可以用于地表水等水系统中微量喹诺酮类抗生素残留的监测。

To establish an HPLC-MS/MS method for the determination of nalidixic acid,pipemidic acid,pefloxacin,ofloxacin,sparfloxacin and gatifloxacin residues in surface water.The surface water samples were randomly collected,filtered,and the pH was adjusted to neutral.The pretreated surface water sample was washed and purified with 10 mL 5%methanol solution on the activated solid-phase extraction column at a flow rate of 8-10 mL/min.the eluent was discarded and drained.Finally,20 mL methanol was used to elute and collect the eluent.The eluent nitrogen was blown to nearly dry,the volume was fixed to 1 mL with acetonitrile,mixed with vortex for 1 min,and determined quantitatively by HPLC-MS/MS.The concentrations of pipemidic acid,ofloxacin,pefloxacin,sparfloxacin,gatifloxacin and nalidixic acid were 0.01-8.00μg/mL.The linear relationship was good in the range,and the correlation coefficientwas greater than 0.995.The detection limits were 1.82,1.39,2.41,1.49,1.93 and 1.12μg/L respectively.The recovery of the method was between 84.2%and 92.2%;the relative standard deviation of repeatability(n=6)was within 5.0%.The experimental results showed that there are the characteristics of fast processing speed and reliable detection results,which can be used to monitor the trace quinolones in surface water and other water systems.