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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。
To establish a method for the simultaneous determination of five macrolide antibiotics (roxithromycin, clarithromycin, azithromycin, spiramycin, and thalidomide) in water by high performance liquid chromatography-tandem mass spectrometry (SPE-MS / MS) Leptin) analysis method. The antibiotics in water samples were enriched by Oasis HLB solid phase extraction cartridges. The mobile phase consisted of C18 column, methanol and 0.1% formic acid as mobile phase, and analyzed by HPLC-MS / MS Multiple reaction monitoring (MRM), internal standard quantification. The recoveries of five macrolide antibiotics ranged from 64.8% to 90.8%. The detection limits were 0.012 ~ 0.085 μg / L and the limits of quantification were 0.041 ~ 0.285 μg / L. The established method was used to detect the residues of five target analytes in the surface water around a chemical industrial park. No tylosin was detected, and the remaining four antibiotics were detected in varying degrees, and the levels of ng / L were detected .