色谱

色谱 ›› 2018, Vol. 36 ›› Issue (4): 370-375.DOI: 10.3724/SP.J.1123.2017.11018

• 研究论文 • 上一篇    下一篇

基于整体柱的固相萃取-高效液相色谱法测定尿液中4种羟基多环芳烃

胡桂羽, 王曼曼, 念琪循, 李娜, 董鑫鑫, 郝玉兰, 王茜, 王学生   

  1. 华北理工大学公共卫生学院, 河北 唐山 063000
  • 收稿日期:2017-11-13 出版日期:2018-04-08 发布日期:2014-02-26
  • 通讯作者: 王茜,E-mail:wwqq517@aliyun.com;王学生E-mail:xswang64@163.com
  • 基金资助:

    国家自然科学基金（21305028）；河北省自然科学基金（H2017209232，H2016209018）；华北理工大学培育基金项目（JQ201717）.

Determination of four hydroxyl polycyclic aromatic hydrocarbons in urine by solid-phase extraction with monolithic column coupled with high performance liquid chromatography

HU Guiyu, WANG Manman, NIAN Qixun, LI Na, DONG Xinxin, HAO Yulan, WANG Qian, WANG Xuesheng   

  1. School of Public Health, North China University of Science and Technology, Tangshan 063000, China
  • Received:2017-11-13 Online:2018-04-08 Published:2014-02-26
  • Supported by:

    National Natural Science Foundation of China (No. 21305028); Natural Science Foundation of Hebei Province (Nos. H2017209232, H2016209018); Training Foundation of North China University of Science and Technology (No. JQ201717).

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摘要：

建立了基于聚合物整体柱的固相萃取-高效液相色谱测定尿液中4种羟基多环芳烃（OH-PAHs）的分析方法。在注射器管中合成聚（甲基丙烯酸丁酯-乙二醇二甲基丙烯酸酯）整体柱（poly （BMA-co-EDMA）），并将其用于尿液中4种羟基多环芳烃的前处理，同时考察了上样浓度、淋洗液、洗脱液和洗脱体积对萃取效率的影响。结合高效液相色谱-荧光分析，4种羟基多环芳烃在各自的范围内线性关系良好（r≥0.9991）；方法的检出限和定量限分别为0.06~0.09 ng/mL和0.20~0.30 ng/mL；日内（n=5）和日间（n=3）精密度分别为1.4%~5.3%和2.6%~7.3%。对焦炉工人尿液样品进行加标（3 ng/mL）回收试验，回收率为78.2%~117.0%。该固相萃取柱能够有效萃取和净化尿液中4种羟基多环芳烃，并且可以重复使用。该法简单、准确，可应用于尿液中羟基多环芳烃的分析。

关键词: 高效液相色谱, 固相萃取, 聚合物整体柱, 尿液, 羟基多环芳烃

Abstract:

A method based on monolithic column solid-phase extraction (SPE) coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous determination of four hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine.A poly (butyl methacrylate-co-ethylene dimethacrylate) monolithic column was prepared in a syringe and was used as the sorbent.The parameters influencing SPE, such as loading volume, washing solvent, eluent, and elution volume, were investigated in detail.Under the optimized conditions, the linearities were obtained in range of 1.2-200.0 ng/mL, and the LODs and LOQs of the analytes were 0.06-0.09 ng/mL and 0.20-0.30 ng/mL, respectively.The intra-day and inter-day relative standard deviations were 1.4%-5.3% and 2.6%-7.3%, respectively.The recoveries evaluated using the spiked (3 ng/mL) urine samples of coke oven workers ranged from 78.2% to 117.0%.The feasibility of the developed method was further demonstrated for the analysis of the real samples.The results indicated that the reusable monolithic column enabled effective purification and enrichment of the four OH-PAHs in urine, and can be applied to the analysis of OH-PAHs in urine due to its simplicity and accuracy.

Key words: high performance liquid chromatography (HPLC), hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs), polymer monolithic column, solid-phase extraction (SPE), urine

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