色谱2017，Vol.35Issue(12)：1245-1250,6.DOI:10.3724/SP.J.1123.2017.09012
超高效液相色谱-高分辨质谱确证分析泥鳅体内五氯酚代谢物
Confirmation and analysis of the metabolites of pentachlorophenol in loaches using ultra-performance liquid chromatography-high resolution mass spectrometry
摘要
Abstract
A method for the characterization of the metabolite pentachlorophenol hydrogen sul-fate(PCP-SO3H)of pentachlorophenol(PCP)in loaches was developed based on ultra-performance liquid chromatography-high resolution mass spectrometry ( UPLC-HRMS ). The loach samples exposed in low concentration of PCP solution were firstly crushed,then extrac-ted by acetonitrile-water solution(70:30,v/v)containing 8%(v/v)triethylamine and purified by mixed anion exchange solid-phase extraction( SPE)cartridges. The chromatographic sepa-ration was carried out on a Waters ACQUITY BEH C18 column(100 mm×2. 1 mm,1. 7 μm). The qualitative analysis of the metabolites of PCP was operated in a negative electrospray ion mode(ESI-)under full mass-data dependent MS2(full mass-ddMS2)mode,and the data of quasi-molecular ion,isotope ions,and MS2 fragmentation ions of metabolites were obtained. The results revealed that the sulfonation was the main metabolic pathway for PCP in loaches, not the hydroxylation or glucuronate pathway. And the metabolite was found to be PCP-SO 3H. Besides,with the increase of exposure time in PCP solution,the concentration of metabolite PCP-SO3H firstly increased;when the exposure time was up to 36 h,the concentration of metabolite in loach reached a maximum value;and then extending the exposure time,the con-centration of PCP-SO3H gradually decreased. When the exposure time was up to 120 h,the con-centration of PCP-SO3H in loaches reached a lowest value,and no significant change occurred for further time. The developed UPLC-HRMS method in this study could be used for the investi-gation of the metabolism of PCP in living beings.关键词
超高效液相色谱-高分辨质谱/五氯酚/代谢物/泥鳅Key words
ultra-performance liquid chromatography-high resolution mass spectrometry ( UPLC-HRMS)/pentachlorophenol( PCP)/metabolite/loach分类
化学化工引用本文复制引用
潘胜东,陈晓红,何仟,李晓海,王立,周健,金米聪..超高效液相色谱-高分辨质谱确证分析泥鳅体内五氯酚代谢物[J].色谱,2017,35(12):1245-1250,6.基金项目
宁波市自然科学基金项目(2016A610178) （2016A610178）
浙江省公共卫生应急检测关键技术重点实验室开放基金项目 （）
宁波市领军和拔尖人才工程.Ningbo Municipal Science Foundation( No. 2016A610178) （ No. 2016A610178）
Opening Foundation of Key Laboratory of Key Technologies of Emergency Detection for Public Health of Zhejiang Province （）
Ningbo Municipal Program for Leading and Top-Notch Talents. （）
