【摘要】 为有效降低磺胺类抗生素测定过程中严重的基质抑制效应，本文将固相萃取、凝胶渗透色谱两种前处理技术结合，建立了一种基于超高效液相色谱-三重四极杆质谱法（UPLC-MS/MS）同时测定环境水样中19种磺胺类抗生素的方法.水样经0.45μm滤膜过滤，调节pH至6并加入Na₂EDTA使其浓度为2.5 mg·L^-1，经Oasis HLB小柱富集，凝胶渗透色谱净化后，采用Hypersil GOLD C₁₈色谱柱（2.1 mm ID×100 mm,1.9μm）分离，以0.05%（V/V）甲酸水溶液和0.05%（V/V）甲酸甲醇溶液梯度洗脱，多反应监测（MRM）模式检测，内标法定量.在最优条件下，19种抗生素的方法检出限（LOD）和定量限（LOQ）分别为0.7—4.4 ng·L^-1和2.8—17.6 ng·L^-1；高中低浓度(10、200、400 ng·L^-1)实际样品加标回收率分别为：低浓度44.5%—102%，中浓度47.7%—97.5%，高浓度51.4%—115%；相对标准偏差分别为：低浓度1.8%—10%，中浓度0.64%—5.9%，高浓度0.71%—4.6%.应用本方法对3个地表水和3个城镇污水处理厂出水进行了测定，共有5种磺胺类抗生素不同程度检出，检出浓度在1.82—3864 ng·L^-1之间.该方法抗基质效应能力强、灵敏度高、精密度好，非常适合环境样品中磺胺类抗生素的测定.更多还原

【Abstract】 To effectively mitigate the inhibitory matrix effects in the determination of sulfonamide antibiotics, a method for the simultaneous determination of 19 sulfonamide antibiotics in environmental aqueous samples was developed. This method combines ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） with two pretreatment techniques:solid-phase extraction（SPE） and gel permeation chromatography（GPC）. Aqueous samples were filtered through 0.45 μm filters, the sample pH was adjusted to 6, and Na₂EDTA was added to achieve a final concentration of 2.5 mg·L^-1. Samples were extracted using Oasis HLB cartridges and subsequently purified through gel permeation chromatography. After pre-concentration, analytes were separated using a Hypersil GOLD C₁₈ column（2.1 mm ID×100 mm, 1.9 μm） with a gradient elution of aqueous and methanolic solutions containing 0.05%（V/V） acetic acid as mobile phases.Detection and quantification were performed in multiple reaction monitoring（MRM） mode using the internal standard method. Under optimal conditions, the method achieved limits of detection（LOD）and quantification（LOQ） ranging from 0.7 —4.4 ng·L^-1 and 2.8 —17.6 ng·L^-1, respectively. The recoveries from actual samples spiked at three levels(10, 200, and 400 ng·L^-1) were 44.5%—102%（low）, 47.7% —97.5%（medium）, and 51.4% —115%（high）. Relative standard deviations（RSDs）ranged from 1.8%—10%（low）, 0.64%—5.9%（medium）, and 0.71%—4.6%（high）. The method was applied to analyze samples from three surface water sites and three urban sewage treatment plants. A total of five sulfonamide antibiotics were detected, with concentrations ranging from 1.82 —3864 ng·L^-1. This method demonstrates strong resistance to matrix effects, high sensitivity, and excellent precision, making it highly suitable for the determination of sulfonamide antibiotics in environmental samples.更多还原