In this article, silver nanoparticles (AgNPs) modified nanofibers that represent a novel kind of packing materials for micro-solid phase extraction (μ-SPE) is reported for the first time. The composite material was fabricated through in-situ formation of AgNPs on the polydopamine (PDA) coated polystyrene electrospun fibers ([email protected]). The nanofibers displayed desirable hydrophilicity, large surface area, high porosity, good extraction ability and certain capacity to resist matrix interference. A μ-SPE combined with liquid chromatography-mass spectrometry (LC–MS) method was developed for the online determination of three monohydroxy polycyclic aromatic hydrocarbons (OH-PAHs) metabolites in human urine. Under the optimal conditions, good linearity (0.02–5 ng mL⁻¹) was acquired with the correlation coefficients (R²) being larger than 0.9962. Low limits of detection (0.007–0.032 ng mL⁻¹) expressed the satisfactory sensitivity of the method. Moreover, the intraday relative standard deviation values lower than 9.7% and the recoveries among the range of 71–116% were obtained. In general, the online μ-SPE-LC–MS method had the features of simplicity, rapidity, sensitivity and automation, and it was expected to become a promising approach for the online analysis of trace OH-PAHs in complex biological samples.

在本文中，首次报道了纳米银（AgNPs）修饰的纳米纤维，它们代表了一种用于微固相萃取（μ-SPE）的新型包装材料。该复合材料是通过在涂有聚多巴胺（PDA）的聚苯乙烯电纺纤维（[受电子邮件保护]）上原位形成AgNP制成的。纳米纤维表现出理想的亲水性，大表面积，高孔隙率，良好的提取能力和一定的抵抗基质干扰的能力。开发了一种μ-SPE与液相色谱-质谱联用（LC-MS）的方法，用于在线测定人尿中的三种单羟基多环芳烃（OH-PAHs）代谢物。在最佳条件下，线性良好（0.02–5 ng mL ^-1）的相关系数（R ²）大于0.9962。低检测限（0.007–0.032 ng mL ^-1）表示该方法具有令人满意的灵敏度。此外，日内相对标准偏差值低于9.7％，回收率在71–116％的范围内。通常，在线μ-SPE-LC-MS方法具有简单，快速，灵敏和自动化的特点，有望成为在线分析复杂生物样品中的痕量OH-PAHs的一种有前途的方法。