超高效液相色谱-串联质谱检测养殖水体中喹诺酮类抗生素

Determination of quinolones in aquaculture waters by ultra performance liquid chromatography-tandem mass spectrometry

建立了一种通过超高效液相色谱-串联质谱法（UPLC-MS/MS）测定养殖水体中14种喹诺酮类药物的方法.水样经甲酸酸化预处理后,采用HLB固相萃取柱富集并净化目标物,以0.2%体积分数的甲酸水溶液-甲醇为流动相,经过梯度洗脱分离,串联质谱多反应监测模式测定,再由外标法定量.结果显示,14种喹诺酮药物浓度为0.5~50.0μg·L-1时线性良好,线性相关系数大于0.995.空白水样在5.00,50.0和100ng·L-13种添加水平下的加标回收率为79.8%~95.4%,相对标准偏差均小于10%.14种喹诺酮药物的检出限为1.00~1.50ng·L-1,定量限为3.50~5.00ng·L-1,结果表明所建立的方法重现性好,灵敏度、回收率高,检测时间短,适用于养殖水体中喹诺酮类药物残留的检测.

A method for the analysis of 14 quinolones residue in aquaculture waters was developed based on ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. After the acidification with formic acid, the water samples were enriched and cleaned-up by HLB solid-phase extraction cartridges. The analytes were separated by UPLC, and detected under Multiple Reaction Monitoring （MRM） mode using 0.2% formic acid （V/V） and methanol as the mobile phase by gradient elution, finally quantified hy the external standard method. Under the optimized conditions, all of the quinolones were in good linearity at the range of 0.5 to 50.0 μg L-1 and the corre- lation coefficients were greater than 0. 995. The averaged recoveries of 14 quinolones at the spiked concentrations of 5.00,50.0,100 ng L-1 were ranged from 79.8% to 95.4% with the relatives standard deviations （n=5）%10%. The limits of the qualitification and quantification of 14 quinolones were from 1.00 to 1.50 ng L-1 and 3.50 to 5.00 ng L-1 , respectively. It is concluded that this method can be successfully applied to the determination of 14 quinolones in aquaculture waters with good reproducibility, high sensitivity, high recovery rate and short analysis time.