摘要
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.
出处
《中国测试》
CAS
北大核心
2017年第3期58-62,共5页
China Measurement & Test
基金
国家863课题(2013AA06A309)
苏州农业职业技术学院青年教师科研能力提升计划资助项目(PPS201304)
关键词
大环内酯类抗生素
固相萃取
高效液相色谱一串联质谱
水体
macrolides antibiotics (MLs)
solid phase extraction (SPE)
high performance liquidchromatography-tandem mass spectrometry(HPLC-MS/MS)
water