固相萃取液相色谱-质谱/质谱联用测定河水中大环内酯类抗生素

应用固相萃取（SPE）及LC—MS／MS技术，建立了水中痕量大环内酯类抗生素即红霉素、脱水红霉素、罗红霉素的分析方法，优化了固相萃取、液相色谱-质谱／质谱等相关条件。水样经HLB固相萃取柱富集净化，以多反应检测方式（MRM）对待测物进行定性和定量分析。3种抗生素在10-2000ng／L范围内具有良好的线性。其定量下限为5ng／L（S／N〉10）。加标纯水和实际水样的回收率在71％-111％之间，相对标准偏差（RSD）在3．7％-8．6％之间。该方法灵敏度高、选择性好、准确度高，适合实际水样中痕量大环内酯类药物的检测。使用该方法测得珠江广州河段某水样中红霉素、脱水红霉素和罗红霉素质量浓度分别为164、291和134ng／L。

Determination of Trace Macrolides in Water Using Solid-phase Extraction and Liquid Chromatography with Tandem Mass Spectrometry

The determination of macrolide antibiotics in water was performed using solid phase extraction(SPE) followed by a combined liquid chromatography(LC) and tandem mass spectrometry(MS/MS) procedure under the multi-reactive model.The experimental results showed that this method was satisfactory for the analysis of several typical antibiotics such as erythromycin(ETM),erythromycin-H_2O(ETM-H_2O) and roxithromycin(RTM) in river water.The linear range was 10-2 000 ng/L and the detection limit was 5 ng/L for ETM,ETMH_2O and RTM.The spiking recoveries for these antibiotics ranged from 71% to 111% and their relative standard deviations(RSD) were less than 8.6%.The concentrations of ETM,ETM-H_2O and RTM measured in Pearl River water(urban Guangzhou) were 164,291 and 134 ng/L,respectively.