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不同水基质中青霉素的同时测定与毒理学评估

Simultaneous determination and toxicological assessment of penicillins in different water matrices.

作者信息

Tong L, Wang Y X, Hermo M Pilar, Barrón D, Barbosa J

机构信息

School of Environmental Studies, China University of Geosciences, Wuhan, 430074, People's Republic of China.

出版信息

Ecotoxicology. 2014 Dec;23(10):2005-13. doi: 10.1007/s10646-014-1336-1. Epub 2014 Sep 4.

Abstract

A multi-residue analysis method was developed for the determination of penicillins in wastewater of WWTP, surface water and groundwater in Spain. The procedure involves a solid phase extraction (SPE) and the subsequent analysis by liquid chromatography coupled to tandem mass spectrometry detection (LC-QqQ-MS/MS). The SPE processes were optimized by test of cartridges, sample pH and elution solvents. ENV+ cartridge was chosen for the extraction of penicillins from different environmental samples. The best conditions for the extraction efficiency of the targets were observed at sample pH 6, by eluting solvents of methanol and acetonitrile respectively. The method has been validated by calibration curve, corresponding regression coefficient, limit of quantification and recoveries. The results showed that the recoveries of more than 90% were presented in all the compounds, except AMOX and AMPI, which had special amino-group in the molecular structure different with others. The matrix effect was also considered in the experiment and it was concluded that different matrix effect could be found between three kinds of waters, and the low retention of AMOX and AMPI on the cartridges was attributed to the matrices interference. The real sample detection showed that the penicillins degraded fast and only AMOX appeared in the studied environmental samples. The results of toxicology test on two compounds (AMOX and AMPI) showed that bacteria V. fischeri was proved to be relatively insensitive to both targets. The decreasing order of toxicity in three environmental waters for AMOX and AMPI was: wastewater > groundwater > surface water.

摘要

开发了一种多残留分析方法,用于测定西班牙污水处理厂废水、地表水和地下水中的青霉素。该程序包括固相萃取(SPE)以及随后通过液相色谱-串联质谱检测(LC-QqQ-MS/MS)进行分析。通过对柱管、样品pH值和洗脱溶剂进行测试,对固相萃取过程进行了优化。选择ENV+柱管用于从不同环境样品中萃取青霉素。在样品pH值为6时,分别用甲醇和乙腈作为洗脱溶剂,观察到目标物萃取效率的最佳条件。该方法已通过校准曲线、相应的回归系数、定量限和回收率进行了验证。结果表明,除阿莫西林(AMOX)和氨苄青霉素(AMPI)外,所有化合物的回收率均超过90%,这两种化合物的分子结构中含有与其他化合物不同的特殊氨基。实验中还考虑了基质效应,得出结论:三种水体之间存在不同的基质效应,阿莫西林和氨苄青霉素在柱管上的低保留率归因于基质干扰。实际样品检测表明,青霉素降解迅速,在所研究的环境样品中仅出现了阿莫西林。对两种化合物(阿莫西林和氨苄青霉素)的毒理学测试结果表明,费氏弧菌对这两种目标物相对不敏感。阿莫西林和氨苄青霉素在三种环境水体中的毒性递减顺序为:废水>地下水>地表水。

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