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Development of sol-gel phenyl/methyl/poly (dimethylsiloxane) sorbent coating for fabric phase sorptive extraction and its application in monitoring human exposure to selected polycyclic aromatic hydrocarbons using high performance liquid chromatography-fluorescence detection
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2020-12-28 , DOI: 10.1016/j.jchromb.2020.122520
Isil Gazioglu , Abuzar Kabir , Ozge S. Zengin , Evrim Kepekci Tekkeli , Kenneth G. Furton , Angela Tartaglia , Marcello Locatelli

Following the convenient, yet very powerful pathway to create designer extraction sorbent using sol-gel chemistry, a novel sol-gel phenyl/methyl/poly(dimethylsiloxane) sorbent coating was created on polyester fabric substrate for fabric phase sorptive extraction (FPSE) and was subsequently applied to monitor human exposure to selected polycyclic aromatic hydrocarbons (PAHs) including pyrene, chrysene, and benzo[a]pyrene in plasma samples obtained from tobacco smoker volunteers using high performance liquid chromatography-fluorescence detector (HPLC-FLD). A rapid FPSE-HPLC-FLD method was developed that adequately resolved the PAHs chromatographically, after their successful extraction from human plasma using fabric phase absorption extraction (FPSE) and subsequently analysed in the liquid chromatographic system by means of an analytical column (InterSustain C-18 column 150 × 4.6 mm, 5 μm) using acetonitrile (ACN) and water as mobile phases in gradient elution mode. With the optimized conditions, the retention times were found to be 6.168, 7.214, and 10.404 min for pyrene, chrysene, and benzo[a]pyrene, respectively. The total chromatographic runtime was limited to 12.5 min.

The method, validated through the calculation of all the analytical parameters according to the International Guidelines, was applied to the analysis of real samples collected from informed volunteers. The proposed approach which included the use of sol-gel phenyl/methyl/poly(dimethylsiloxane) immobilized on hydrophobic polyester substrate and C18 stationary phase used in HPLC, has shown a high potential as a rapid tool for future clinical, forensic and toxicological applications, also in the light of the LOD and LOQ values comparable to those normally obtainable with more sophisticated, and expensive instruments that often require highly trained personnel. The results reported here further consolidate the application of FPSE in the analysis of biological samples for both diagnostic and analytical-clinical purposes.



中文翻译:

用于织物相吸附萃取的溶胶-凝胶苯基/甲基/聚(二甲基硅氧烷)吸附剂涂层的开发及其在使用高效液相色谱-荧光检测技术监测人暴露于选定的多环芳烃中的应用

遵循使用溶胶-凝胶化学方法创建设计师提取吸附剂的便捷但功能强大的途径,在聚酯织物基材上创建了一种新型的溶胶-凝胶苯基/甲基/聚(二甲基硅氧烷)吸附剂涂层,用于织物相吸附萃取(FPSE)。随后应用高效液相色谱-荧光检测器(HPLC-FLD)监测人体接触自吸烟者志愿者的血浆样品中所选的多环芳烃(PAH),包括pyr,including和苯并[a] py。开发了一种快速的FPSE-HPLC-FLD方法,可通过色谱法充分分离PAH,使用织物相吸收萃取(FPSE)从人血浆中成功提取后,随后在液相色谱系统中通过使用乙腈(ACN)和水的分析柱(InterSustain C-18色谱柱150×4.6 mm,5μm)进行分析作为梯度洗脱模式下的流动相。在优化的条件下,发现pyr,和苯并[a] py的保留时间分别为6.168、7.214和10.404分钟。总色谱运行时间限制为12.5分钟。

通过根据《国际准则》计算所有分析参数进行验证的方法适用于分析从知情志愿者那里收集的真实样品。所提议的方法包括将溶胶-凝胶苯基/甲基/聚(二甲基硅氧烷)固定在疏水性聚酯基质上以及用于HPLC的C18固定相的使用,已显示出作为未来临床,法医和毒理学应用的快速工具的巨大潜力,鉴于LOD和LOQ值可与通常需要训练有素的人员使用更复杂,更昂贵的仪器通常可获得的值相比较。此处报道的结果进一步巩固了FPSE在用于诊断和分析临床目的的生物样品分析中的应用。

更新日期:2021-01-10
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