固相萃取-高效液相色谱-串联质谱测定水中5种大环内酯类抗生素

Simultaneous determination of 5 macrolides antibiotics in natural water samples using solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

建立固相萃取(SPE)、高效液相色谱-串联质谱(HPLC-MS/MS)同时测定水中5种大环内酯类抗生素(罗红霉素、克拉霉素、阿奇霉素、螺旋霉素和泰乐菌素)的分析方法。水样中的抗生素通过Oasis HLB固相萃取小柱富集后,以C18反相色谱柱为分析柱,甲醇和0.1%甲酸水溶液为流动相,采用HPLC-MS/MS进行定量分析,检测方式为多反应监测模式(MRM),内标法定量。5种大环内酯类抗生素的回收率在64.8%~90.8%之间,仪器检出限为0.012~0.085μg/L,定量限为0.041~0.285μg/L。将建立的方法用于检测某化学工业园区周边地表水中5种目标分析物的残留,均未检测到泰乐菌素,其余4种抗生素均有不同程度检出,检出浓度在ng/L水平。

A method with solid phase extraction（SPE） and high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was developed for the determination of five macrolides（roxithromycin, clarithromycin, azithromycin, spiramycin and tylosin） in natural water samples.The macrolides were extracted from water samples using Oasis HLB cartridges and then separatedon a reverse phase column using methanol and 0.1% formic acid as mobile phases. The macrolideswere quantified with the internal standard method under multiple reaction monitoring（MRM） mode.The recoveries of the five macrolides ranged from 64.8% to 90.8%. The instrumental limits ofdetection and quantification are 0.012-0.085 μg/L and 0.041-0.285 μg/L respectively. Only Tylosinwas not found by the proposed method in the studied rivers surrounding a Chemical IndustryPark, while the other four macrolides were detected at the ng/L level.