色谱

色谱 ›› 2019, Vol. 37 ›› Issue (3): 252-258.DOI: 10.3724/SP.J.1123.2018.10023

• 研究快报 • 上一篇    下一篇

基于氮化碳复合材料磁性固相萃取结合高效液相色谱法测定尿液中3种羟基多环芳烃

念琪循, 刘园满, 孙冰, 王曼曼   

  1. 华北理工大学公共卫生学院, 河北 唐山 063210
  • 收稿日期:2018-10-08 出版日期:2019-03-08 发布日期:2015-01-21
  • 通讯作者: 王曼曼.E-mail:mmwangheuu@126.com.
  • 基金资助:

    河北省自然科学基金（H2017209232，H2016209018）；河北省教育厅研究项目（ZD2018014）；华北理工大学培育基金项目（JQ201717）；华北理工大学研究生创新项目（2019S11）.

Determination of three hydroxyl polycyclic aromatic hydrocarbons in urine using magnetic solid-phase extraction with magnetic carbon nitride composites coupled with high performance liquid chromatography

NIAN Qixun, LIU Yuanman, SUN Bing, WANG Manman   

  1. School of Public Health, North China University of Science and Technology, Tangshan 063210, China
  • Received:2018-10-08 Online:2019-03-08 Published:2015-01-21
  • Supported by:

    Natural Science Foundation of Hebei Province (Nos. H2017209232, H2016209018); Research Foundation of Education Bureau of Hebei Province (No. ZD2018014); Training Foundation of North China University of Science and Technology (No. JQ201717); Graduate Student Innovation Fund of North China University of Science and Technology (No. 2019S11).

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摘要：

建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料，经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后，用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积（单次洗脱体积×洗脱次数）对萃取效率的影响。结合高效液相色谱-荧光分析，在0.25~250 μg/L范围内线性关系良好（相关系数r=0.999），3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L，回收率为90.1%~102%，日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效，可用于尿液中羟基多环芳烃的分析。

关键词: 磁性氮化碳材料, 磁性固相萃取, 高效液相色谱, 尿液, 羟基多环芳烃

Abstract:

A method based on the magnetic solid-phase extraction using magnetic carbon nitride composites coupled with high performance liquid chromatography-fluorescence detector (HPLC-FLD) was developed for the simultaneous determination of three hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine. The synthesized sorbent was characterized by scanning electron microscope, X-ray diffractometer, vibrating sample magnetometer and surface area analyzer. The extraction parameters such as amount of sorbent, extraction time, eluting solvent and volume (single eluting volume×eluting times) were investigated in detail. Under the optimized conditions, the method showed a linear range of 0.25-250 μg/L (correlation coefficient=0.999). The limit of detection was 0.08 μg/L and the limit of quantification was 0.25 μg/L for each analyte. The proposed method gave a recovery of 90.1%-102%. The relative standard deviations for the intra-day and inter-day were 1.5%-7.7% and 2.2%-8.7%, respectively. The feasibility of the developed method was further demonstrated during the analysis of real samples. The results indicate that the magnetic carbon nitride composites can be used for the effective purification and enrichment of three OH-PAHs in urine. In addition, the method can be applied for analysis of urinary OH-PAHs in a simple, fast, and effective manner.

Key words: high-performance liquid chromatography (HPLC), hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs), magnetic carbon nitride (g-C3N4) composite, magnetic solid-phase extraction (MSPE), urine

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