Qian Liangliang, Li Ruixian, Di Qiannan, Shen Yang, Xu Qian, Li Jian
Key Laboratory of Environmental Medicine Engineering, Ministry of Education, School of Public Health, Southeast University, Nanjing 210009, China.
Department of Obstetrics and Gynecology, Zhong Da Hospital, School of Medicine, Southeast University, Nanjing 210009, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 1;1061-1062:146-152. doi: 10.1016/j.jchromb.2017.07.004. Epub 2017 Jul 31.
A method was established for the analysis of nonylphenol (NP) in rat urine samples based on a solid-phase extraction (SPE) procedure with an amino functionalized polyacrylonitrile nanofibers mat (NH-PAN NFM) as sorbent coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The calibration curves prepared in three different days showed good linearity over a wide range of NP concentrations from 0.1 to 100.0ng/mL. It was remarkable that the proposed NH-PAN NFsM based SPE method showed superior extraction efficiency with the consumption of only 4mg of sorbent and 500μL of eluent. The eluent without any further concentration was directly analyzed by HPLC-MS/MS. As a result, a simple and effective sample preparation was achieved. In addition, the notable lower detection limit (LOD) of 0.03ng/mL revealed the excellent sensitivity of the proposed method in comparison with that in literatures. The recoveries ranged from 85.0% to 114.8% with the relative standard deviations (RSDs) ranging from 7.5% to 13.7%, which were better than or comparable to those from the published methods, suggesting high accuracy of the proposed method. The proposed method was applied in primary study on the disposition of nonylphenol after long-term low-level exposure in rats, providing information for health risk assessment on the real scenarios of NP exposure. NH-PAN NFsM shows great potential as a novel SPE sorbent for the analysis of biological samples.
建立了一种基于固相萃取(SPE)的方法,以氨基功能化聚丙烯腈纳米纤维毡(NH-PAN NFM)为吸附剂,结合高效液相色谱-串联质谱(HPLC-MS/MS)分析大鼠尿液样本中的壬基酚(NP)。在三天内制备的校准曲线在0.1至100.0 ng/mL的宽NP浓度范围内显示出良好的线性。值得注意的是,所提出的基于NH-PAN NFsM的SPE方法仅消耗4 mg吸附剂和500 μL洗脱液,就显示出优异的萃取效率。无需进一步浓缩的洗脱液直接通过HPLC-MS/MS进行分析。结果,实现了一种简单有效的样品制备方法。此外,0.03 ng/mL的显著较低检测限表明该方法与文献中的方法相比具有出色的灵敏度。回收率在85.0%至114.8%之间,相对标准偏差(RSD)在7.5%至13.7%之间,优于或与已发表方法相当,表明该方法具有较高的准确性。该方法应用于大鼠长期低水平暴露后壬基酚处置的初步研究,为NP暴露实际场景的健康风险评估提供信息。NH-PAN NFsM作为一种用于生物样品分析的新型SPE吸附剂具有巨大潜力。