超高效液相色谱串联质谱法同时测定城市污水处理厂污泥中12种抗生素

Simultaneous determination of 12 antibiotics in sewage sludge by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

建立了一种固相萃取-超高效液相色谱-串联质谱法同时测定污泥中4类12种抗生素的方法.采用SAX串联Oasis HLB固相萃取柱净化富集污泥样品中的抗生素,选定p H 3、洗脱体积8 m L作为最佳前处理条件.采用超高效液相色谱-串联质谱检测抗生素样品,以0.3%的甲酸和乙腈作为流动相,经梯度洗脱进行分离,在多反应检测模式下进行测定.经测定,污泥样品中磺胺类抗生素、脱水红霉素和罗红霉素平均回收率为50%—80%,其余抗生素的平均回收率为82%—119%,12种抗生素在污泥中的定量限为0.001—0.008μg·kg^(-1)dw.并用该法对天津市某污水处理厂污泥样品进行检测,证明该方法可满足实际检测要求.

A method for the determination of 12 antibiotics in sewage sludge was developed using solid-phase extraction and ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry （SPE-UPLC-MS/MS）. The antibiotics in sludge samples were enriched and purified by SAX and Oasis HLB solid-phase extraction columns. The optimal pretreatment conditions of pH 3 and 8 mL elution volume were selected. All antibiotics were detected by UPLC-MS/MS in a multiple reaction monitoring mode, separated by gradient elution with the mobile phase of 0.3% formic acid and acetonitrile. Results show that the average recovery efficiencies of sulfonamide antibiotics, erythromycin and roxithromycin in sludge samples were 50%--80%, and the average recovery efficiencies of the other antibiotics were 82%--119%. The quantitative limit of the 12 antibiotics was 0.001--0.008 μg· kg-1 dry weight in sludge. The method was utilized for the sludge samples from a wastewater treatment plant in Tianjin, suggesting this method meets the practical detection application.