Hubei Province Key Laboratory of Occupational Hazard Identification and Control, School of Public Health, Wuhan University of Science and Technology, Wuhan, P. R. China.
Hubei Key Laboratory of Nutritional Quality and Safety of Agro-products, Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Sciences, Wuhan, P. R. China.
J Sep Sci. 2022 Mar;45(6):1262-1272. doi: 10.1002/jssc.202100830. Epub 2022 Jan 24.
In this work, a simple and miniaturized solid-phase extraction device was constructed by connecting a commercial nylon needle filter to a syringe, which was applied for extracting 1-hydroxypyrene from a urine sample via hydrophobic and hydrogen bond interactions. The nylon membrane in the needle filter acted as the solid-phase extraction adsorbent, meanwhile, it filtered the particles in the urine sample. To obtain high extraction efficiency, key parameters influencing extraction recovery were investigated. The entire pretreatment process was accomplished within 5 min under the optimal conditions. By coupling high-performance liquid chromatography-ultraviolet, a rapid, low-cost, and convenient nylon needle filter-based method was established for the analysis of 1-hydroxypyrene in a complex urine matrix. Within the linearity range of 0.2-1000 μg/L, the method exhibited a satisfactory correlation coefficient (R = 0.9999). The limit of detection was 0.06 μg/L, and the recoveries from urine sample spiked with three concentrations (5, 20, and 100 μg/L) ranged from 105.8% to 113.1% with the relative standard deviations less than 6.7% (intra-day, n = 6) and 8.9% (inter-day, n = 4). Finally, the proposed method was successfully applied for detecting 1-hydroxypyrene in urine samples from college students, smokers, gas station workers, and chip factory workers. The detected concentration in actual urine samples ranged from 0.46 to 5.26 μg/L. Taken together, this simple and cost-effective nylon needle filter-based solid-phase extraction device showed an excellent application potential for pretreating hydrophobic analytes from aqueous samples.
在这项工作中,通过将商业尼龙针式过滤器连接到注射器上,构建了一种简单且微型化的固相萃取装置,通过疏水和氢键相互作用,从尿液样品中萃取 1-羟基芘。针式过滤器中的尼龙膜作为固相萃取吸附剂,同时过滤尿液样品中的颗粒。为了获得高萃取效率,研究了影响萃取回收率的关键参数。在最佳条件下,整个预处理过程在 5 分钟内完成。通过将高效液相色谱-紫外光谱法相耦合,建立了一种快速、低成本且方便的基于尼龙针式过滤器的方法,用于分析复杂尿液基质中的 1-羟基芘。在线性范围为 0.2-1000 μg/L 时,该方法表现出令人满意的相关系数(R = 0.9999)。检测限为 0.06 μg/L,从尿液样品中以三个浓度(5、20 和 100 μg/L)添加时的回收率范围为 105.8%至 113.1%,日内相对标准偏差小于 6.7%(n = 6),日间相对标准偏差小于 8.9%(n = 4)。最后,该方法成功应用于检测大学生、吸烟者、加油站工作人员和芯片厂工作人员尿液样品中的 1-羟基芘。实际尿液样品中的检测浓度范围为 0.46-5.26 μg/L。总之,这种简单且经济高效的基于尼龙针式过滤器的固相萃取装置显示出了从水性样品中预处理疏水性分析物的优异应用潜力。