法医学杂志

法医学杂志 ›› 2024, Vol. 40 ›› Issue (1): 30-36.DOI: 10.12116/j.issn.1004-5619.2022.320301

• 论著 • 上一篇    下一篇

地表水中34种新兴污染物的超高效液相色谱-四极杆-飞行时间质谱快速筛查

吕琛山1,2,3(), 曹艺璇1,2,3, 穆哓茜1,2,3, 崔海燕1,2,3, 王涛1,2,3, 尉志文1,2,3, 贠克明1,2,3(), 胡萌1,2,3()   

  1. 1.山西医科大学法医学院，山西 晋中 030600
    2.法医学山西省重点实验室，山西 晋中 030600
    3.法庭毒物分析公安部重点实验室，山西 晋中 030600
  • 收稿日期:2022-03-07 发布日期:2024-03-19 出版日期:2024-02-25
  • 通讯作者: 贠克明,胡萌
  • 作者简介:吕琛山（1995—），男，硕士研究生，主要从事法医毒物分析和环境污染物分析研究；E-mail：lvchenshan2210@163.com
  • 基金资助:
    国家自然科学基金资助项目(21806095);国家重点研发计划资助项目(2017YFC0803504)

Rapid Screening of 34 Emerging Contaminants in Surface Water by UHPLC-Q-TOF-MS

Chen-shan LÜ1,2,3(), Yi-xuan CAO1,2,3, Xiao-xi MU1,2,3, Hai-yan CUI1,2,3, Tao WANG1,2,3, Zhi-wen WEI1,2,3, Ke-ming YUN1,2,3(), Meng HU1,2,3()   

  1. 1.School of Forensic Medicine, Shanxi Medical University, Jinzhong 030600, Shanxi Province, China
    2.Shanxi Key Laboratory of Forensic Medicine, Jinzhong 030600, Shanxi Province, China
    3.Key Laboratory of Forensic Toxicology of Ministry of Public Security, Jinzhong 030600, Shanxi Province, China
  • Received:2022-03-07 Online:2024-03-19 Published:2024-02-25
  • Contact: Ke-ming YUN, Meng HU

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摘要：

目的 建立基于超高效液相色谱-四极杆-飞行时间质谱（ultra-high performance liquid chromatography- quadrupole-time of flight mass spectrometry，UHPLC-Q-TOF-MS）技术快速筛查地表水中34种新兴污染物的方法。 方法 通过正交试验设计优化固相萃取（solid phase extraction，SPE）前处理条件，样品经Oasis® HLB和Oasis® MCX固相萃取柱串联富集萃取。萃取物采用Kinetex® EVO C18色谱柱分离，0.1%甲酸水溶液和0.1%甲酸甲醇溶液梯度洗脱，Q-TOF-MS “fullscan”和“targeted MS/MS”模式检测34种新兴污染物，建立34种新兴污染物母离子、子离子及保留时间的数据库。 结果 地表水中34种新兴污染物在各自线性范围内呈良好的线性关系，相关系数（r）大于0.97。检出限为0.2~10 ng/L，回收率为81.2%~119.2%，日间精密度为0.78%~18.70%。将方法应用于多份地表水样品的检测，共检出6种新兴污染物，质量浓度为1.93~157.71 ng/L。 结论 该方法能简单、快速地对地表水中的多种痕量级新兴污染物进行筛查分析。

关键词: 法医学, 毒物化学, 固相萃取, 超高效液相色谱-四极杆-飞行时间质谱, 地表水, 新兴污染物

Abstract:

Objective To establish a rapid screening method for 34 emerging contaminants in surface water by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry （UHPLC-Q-TOF-MS）. Methods The pretreatment conditions of solid phase extraction （SPE） were optimized by orthogonal experimental design and the surface water samples were concentrated and extracted by Oasis® HLB and Oasis® MCX SPE columns in series. The extracts were separated by Kinetex® EVO C18 column， with gradient elution of 0.1% formic acid aqueous solution and 0.1% formic acid methanol solution. Q-TOF-MS ‘fullscan’ and ‘targeted MS/MS’ modes were used to detect 34 emerging contaminants and to establish a database with 34 emerging contaminants precursor ion， product ion and retention times. Results The 34 emerging contaminants exhibited good linearity in the concentration range respectively and the correlation coefficients （r） were higher than 0.97. The limit of detection was 0.2-10 ng/L and the recoveries were 81.2%-119.2%. The intra-day precision was 0.78%-18.70%. The method was applied to analyze multiple surface water samples and 6 emerging contaminants were detected， with a concentration range of 1.93-157.71 ng/L. Conclusion The method is simple and rapid for screening various emerging contaminants at the trace level in surface water.

Key words: forensic medicine, toxicology, solid phase extraction, ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry, surface water, emerging contaminants

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