色谱

色谱 ›› 2017, Vol. 35 ›› Issue (12): 1245-1250.DOI: 10.3724/SP.J.1123.2017.09012

• 研究论文 • 上一篇    下一篇

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

潘胜东1, 陈晓红1, 何仟2, 李晓海1, 王立1, 周健1, 金米聪1   

  1. 1. 宁波市疾病预防控制中心, 浙江省微量有毒化学物健康风险评估技术研究重点实验室, 宁波市毒物研究与控制重点实验室, 浙江 宁波 315010;
    2. 中国疾病预防控制中心, 职业卫生与中毒控制所, 北京 100050
  • 收稿日期:2017-09-06 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 金米聪,E-mail:jmcjc@163.com
  • 基金资助:

    宁波市自然科学基金项目（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.

Confirmation and analysis of the metabolites of pentachlorophenol in loaches using ultra-performance liquid chromatography-high resolution mass spectrometry

PAN Shengdong1, CHEN Xiaohong1, HE Qian2, LI Xiaohai1, WANG Li1, ZHOU Jian1, JIN Micong1   

  1. 1. Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China;
    2. National Institute of Occupational Health and Poison Control, Chinese Municipal Center for Disease Control and Prevention, Beijing 100050, China
  • Received:2017-09-06 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Ningbo Municipal Science Foundation (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.

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160

被引次数

2

摘要：

建立了超高效液相色谱-高分辨质谱（UPLC-HRMS）鉴定泥鳅体内五氯酚代谢物五氯酚磺酸酯的方法。将在低浓度五氯酚下暴露的泥鳅样品粉碎，采用含8%（体积分数）三乙胺的70%（体积分数）乙腈水溶液提取，经混合阴离子交换小柱萃取净化，在ACQUITY BEH C18色谱柱（100 mm×2.1 mm，1.7 μm）上分离，采用电喷雾负离子（ESI-）一级质谱全扫描加数据依赖的二级质谱扫描（full mass-ddMS2）模式测定，获得代谢物的准分子离子、同位素离子和二级质谱碎片离子的精确质量数。结果表明，五氯酚在泥鳅体内的代谢以磺化为主，没有发现羟基化和葡萄糖醛酸化。代谢物主要为五氯酚磺酸酯，其含量随着暴露时间（t）的延长逐渐增加，当暴露时间为36 h时达到峰值，随后逐渐减小，当t ≥ 120 h时，五氯酚磺酸酯含量基本维持不变。该方法可用于生物体内五氯酚的代谢研究。

关键词: 超高效液相色谱-高分辨质谱, 代谢物, 泥鳅, 五氯酚

Abstract:

A method for the characterization of the metabolite pentachlorophenol hydrogen sulfate (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 extracted 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 separation 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-SO3H. 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 concentration of PCP-SO3H gradually decreased. When the exposure time was up to 120 h, the concentration 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 investigation of the metabolism of PCP in living beings.

Key words: loach, metabolite, pentachlorophenol (PCP), ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS)

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