Bezmialem Vakif University, Faculty of Pharmacy, Department of Analytical Chemistry, Fatih, 34093 Istanbul, Turkey.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, 11200 SW 8th St, Miami, FL 33199, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Jan 15;1163:122520. doi: 10.1016/j.jchromb.2020.122520. Epub 2020 Dec 28.
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.
采用简便而强大的溶胶-凝胶化学方法，成功制备了新型苯基/甲基/聚（二甲基硅氧烷）溶胶-凝胶萃取剂，并将其涂覆在聚酯纤维基底上，用于纤维相固相萃取（FPSE），随后应用于监测吸烟志愿者血浆中多环芳烃（PAHs）的暴露情况，包括芘、䓛和苯并[a]芘。采用高效液相色谱-荧光检测法（HPLC-FLD）对样品进行分析。建立了一种快速的 FPSE-HPLC-FLD 方法，该方法能够充分分离 PAHs，成功地从人血浆中提取 PAHs 后，采用纤维相吸收萃取（FPSE）进行萃取，然后在液相色谱系统中通过分析柱（InterSustain C-18 柱，150×4.6mm，5μm），以乙腈（ACN）和水为流动相进行梯度洗脱。在优化的条件下，芘、䓛和苯并[a]芘的保留时间分别为 6.168、7.214 和 10.404min。总色谱运行时间限制在 12.5min 以内。该方法通过根据国际指南计算所有分析参数进行了验证，并应用于从知情志愿者采集的真实样本的分析。所提出的方法包括使用固定在疏水性聚酯基底上的溶胶-凝胶苯基/甲基/聚（二甲基硅氧烷）和 HPLC 中使用的 C18 固定相，已显示出作为未来临床、法医和毒理学应用的快速工具的高潜力，这也考虑到了检测限和定量限值与通常使用更复杂、昂贵的仪器获得的值相当，这些仪器通常需要高度训练有素的人员。这里报告的结果进一步巩固了 FPSE 在生物样品分析中的应用，无论是用于诊断还是分析临床目的。
