关键词: automated solid-phase extraction environmental water isotope dilution sulfonamide antimicrobials ultra-high performance liquid chromatography–tandem mass spectrometry

Mesh : Humans Tandem Mass Spectrometry / methods Water Chromatography, High Pressure Liquid / methods Chromatography, Liquid Sulfanilamide Anti-Infective Agents / analysis Sulfonamides / analysis Solid Phase Extraction / methods

来  源:   DOI:10.3390/molecules28124694   PDF(Pubmed)

Abstract:
The large-scale use of sulfonamide antimicrobials in human and veterinary medicine has seriously endangered the ecological environment and human health. The objective of this study was to develop and validate a simple and robust method for the simultaneous determination of seventeen sulfonamides in water using ultra-high performance liquid chromatography-tandem mass spectrometry coupled with fully automated solid-phase extraction. Seventeen isotope-labeled internal standards for sulfonamides were used to correct matrix effects. Several parameters affecting extraction efficiency were systematically optimized, and the enrichment factors were up to 982-1033 and only requiring about 60 min per six samples. Under the optimized conditions, this method manifested good linearity (0.05-100 μg/L), high sensitivity (detection limits: 0.01-0.05 ng/L), and satisfactory recoveries (79-118%) with acceptable relative standard deviations (0.3-14.5%, n = 5). The developed method can be successfully utilized for the determination of 17 sulfonamides in pure water, tap water, river water, and seawater. In total, six and seven sulfonamides were detected in river water and seawater, respectively, with a total concentration of 8.157-29.676 ng/L and 1.683-36.955 ng/L, respectively, and sulfamethoxazole was the predominant congener.
摘要:
磺胺类抗菌药物在人兽医学中的大量使用,严重危害了生态环境和人类健康。本研究的目的是开发并验证一种简单而可靠的方法,该方法使用超高效液相色谱-串联质谱结合全自动固相萃取同时测定水中的17种磺胺类药物。使用了十七个同位素标记的磺胺类内标来校正基体效应。对影响提取效率的几个参数进行了系统的优化,富集因子高达982-1033,每6个样品仅需要约60分钟。在优化条件下,该方法表现出良好的线性(0.05-100μg/L),高灵敏度(检测限:0.01-0.05ng/L),和令人满意的回收率(79-118%),可接受的相对标准偏差(0.3-14.5%,n=5)。该方法可用于纯净水中17种磺胺类药物的测定,自来水,河水,和海水。总的来说,在河水和海水中检测到六种和七种磺胺类药物,分别,总浓度为8.157-29.676ng/L和1.683-36.955ng/L,分别,磺胺甲恶唑是主要的同源物。
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