色谱2025，Vol.43Issue(8)：915-925,11.DOI:10.3724/SP.J.1123.2024.08001
在线固相萃取净化-超高效液相色谱-串联质谱法测定海洋沉积物中22种抗生素
Determination of 22 antibiotics in marine sediments by online solid-phase extraction purification-ultra-high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
This study developed a novel method for the detection of 22 antibiotics in marine sediments by integrating online solid-phase extraction(SPE)with ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The method was subsequently applied to the analytical determination of antibiotics in offshore bay sediments.Optimal experimental conditions were established through systematic optimization of sample extraction and online SPE parameters.Sediment samples were extracted using an acetonitrile-EDTA/McIlvaine buffer solution(1:1,v/v),diluted with ultrapure water,and then purified and enriched using a large-pore styrene/divinylbenzene-packed PLRP-S online SPE column.The processed samples were separated on a Poroshell EC-C18 column(50 mm×2.1 mm,1.9 µm)and detected in electrospray ionization(ESI)positive ion mode with multiple reaction monitoring(MRM)acquisition.The entire analytical process was completed within 14 min.The results showed that the 22 antibiotics showed good linearity in their respective mass concentration ranges with the correlation coefficients(R2)≥0.990 0,the limits of detection(LODs,S/N=3)were 0.001-0.08 ng/g,and the limits of quantification(LOQs,S/N=10)were 0.004-0.4 ng/g.The spiked recoveries of the 22 antibiotics under three spiked levels(low,medium and high)were 45.1％-145.6％with the relative standard deviations(RSDs)<14％.The method was used to detect antibiotics in winter and summer sediment samples from Shandong Sishili Bay offshore.The results showed that a total of 19 antibiotics from five classes were detected in nine summer sediment samples,with the contents ranging from 0.01 to 34.64 ng/g;and oxytetracycline exhibited the highest detection level.A total of 20 antibiotics from five classes were detected in 10 winter sediment samples,with the contents ranging from 0.004-19.11 ng/g;and ofloxacin showed the highest detection level.Compared with the commonly used offline SPE method,this method greatly simplifies the sample purification process and provides a simple and effective method for the routine detection of common antibiotics in marine sediments.关键词
在线固相萃取/超高效液相色谱-串联质谱/沉积物/抗生素/四十里湾Key words
online solid-phase extraction(SPE)/ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)/sediments/antibiotics/Sishili Bay分类
化学化工引用本文复制引用
王兰香,陈军辉,盛璨璨,范圣晴,何秀平,李先国..在线固相萃取净化-超高效液相色谱-串联质谱法测定海洋沉积物中22种抗生素[J].色谱,2025,43(8):915-925,11.基金项目
国家自然科学基金-山东联合基金(U2106205).National Natural Science Foundation of China-Shandong Joint Fund(No.U2106205). （U2106205）
