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采用大体积直接进样液相色谱-串联质谱法同时分析瓶装水中的多类抗生素。

Simultaneous analysis of multi-class antibiotics in bottled water using large-volume direct-injection LC-MS/MS.

作者信息

Wang Haijun, Zhang Qiao, Li Xiaolin, Chen Huan, Zhu Xiaolan, Yang Liming, Yin Hongling, Sun Jing, Fang Shuhong, Zhang Hui

机构信息

College of Resources and Environment, Chengdu University of Information Technology Chengdu 610225 China

Department of Environmental Engineering and Earth Science, Clemson University South Carolina 29634 USA.

出版信息

RSC Adv. 2025 May 20;15(21):16973-16982. doi: 10.1039/d5ra01764e. eCollection 2025 May 15.

Abstract

A large-volume direct-injection (LVDI) method was developed and validated for the simultaneous analysis of 69 antibiotics in bottled water using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Target antibiotics included 23 sulfonamides, 19 quinolones, 12 macrolides, 11 β-lactams, and 4 tetracyclines. Optimization of ion source parameters led to enhanced signal intensities for 55 antibiotics. The 100 μL injection volume was both feasible and preferred, resulting in increased signal intensities while maintaining unchanged peak shapes for the antibiotics. Good absolute recoveries for the 69 antibiotics were obtained with the LVDI method, primarily ranging from 80% to 120%, whereas lower absolute recoveries of macrolides, quinolones, sulfonamides and β-lactams were observed with a solid-phase extraction (SPE) method. The limits of detection (LODs) for antibiotics were generally comparable between the LVDI and SPE methods, with values below 1 ng L for most antibiotics (0.00271-26.6 ng L). Analysis of 25 brands of bottled water using the LVDI method revealed the presence of 54 antibiotics from 5 classes, with detection frequencies (DFs) ranging from 4% to 100% and detected concentrations between 0.0453 and 37.4 ng L. Multiple antibiotics were detected simultaneously in bottled water, with more than 10 antibiotics identified in each of 9 different brands. Quinolones and sulfonamides were the predominant antibiotics, accounting for over 80% of the total concentration. Only sulfaclozine showed significantly different concentrations between purified drinking water and natural mineral water (22.2 17.2 ng L, < 0.05).

摘要

开发并验证了一种大体积直接进样(LVDI)方法,用于使用超高效液相色谱-串联质谱(UHPLC-MS/MS)同时分析瓶装水中的69种抗生素。目标抗生素包括23种磺胺类、19种喹诺酮类、12种大环内酯类、11种β-内酰胺类和4种四环素类。离子源参数的优化提高了55种抗生素的信号强度。100 μL进样体积既可行又更优,可增加信号强度,同时保持抗生素的峰形不变。LVDI方法对69种抗生素具有良好的绝对回收率,主要范围为80%至120%,而固相萃取(SPE)方法对大环内酯类、喹诺酮类、磺胺类和β-内酰胺类的绝对回收率较低。LVDI和SPE方法对抗生素的检测限(LOD)总体相当,大多数抗生素的值低于1 ng/L(0.00271 - 26.6 ng/L)。使用LVDI方法分析25个品牌的瓶装水发现存在来自5类的54种抗生素,检测频率(DF)范围为4%至100%,检测浓度在0.0453至37.4 ng/L之间。瓶装水中同时检测到多种抗生素,9个不同品牌中的每一个都鉴定出10种以上的抗生素。喹诺酮类和磺胺类是主要抗生素,占总浓度的80%以上。仅磺胺氯嗪在纯净水和天然矿泉水中的浓度存在显著差异(22.2±17.2 ng/L,P<0.05)。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4996/12091094/0b4e34477325/d5ra01764e-f1.jpg

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