目的:建立了同时测定水产养殖沉积物中22种抗生素的通过式固相萃取柱/超高效液相色谱-串联质谱法.方法:样品用8 mL EDTA-Mcllvaine-乙腈=4:4超声提取,提取液过HLB通过式固相柱净化,UPLC-MS/MS检测,基质工作曲线和同位素内标法同时定量.结果:在2.00～100μg/L范围内,22种抗生素的线性关系良好,相关系数均大于0.998.在10μg/kg、50μg/kg、100μg/kg这3个添加水平下,重复测定6次,回收率在60.3％～109.7％,相对标准偏差为1.2％～13.2％,符合GB/T 27404—2008对回收率和精密度的要求.结论:该方法高效快捷,准确可靠,适用于沉积物中抗生素类药物的快速测定.
Simultaneous Determination of Sulfonamides, Quinolones and Tetracycline 22 Antibiotics Residues in Aquaculture Sediments Using Solid-Phase Extraction Column/ultra-High Performance Liquid Chromatography-tandem Mass Spectrometry
Objective: The method for simultaneous determinatiom of 22 antibiotics residues in sediment from aquaculture environment by using ultra high performance liquid chromatography-mass spectrometry (UPLC-MS/MS)in combination with pass-through column was established. Method: The samples were extracted by ultrasonic with 8 mL EDTA-Mcllvaine and acetonitrile equal to 4:4,and purified by HLB pass-through solid phase column. After purification, the samples were analyzed by UPLC-MS/MS, and the samples were quantified simultaneous by matrix working curve and isotope internal standard method. Results:There was a good linear relationship in the range of 2.00～100 μg/L , with R greater than 0.998. The recoveries were in the range of 60.3％～109.7％,and the RSD was in the range of 1.2％～13.2％ at 10 μg/kg, 50 μg/kg and 100 μg/kg supplemental levels for six times, which met the requirements of recoveries and precision for GB/T 27404—2008. Conclusion: The method is efficient, fast, accurate and reliable. It is suitable for the fast determination of the antibi-otics in sediment.
UPLC-MS/MSsedimentantibioticsmatrix working curveisotopeinternal standard
万方数据
维普
