Chemistry Department, College of Science, Shahid Chamran University of Ahvaz, Ahvaz, 61357-43337, Iran.
Faculty of Pharmacy, Ahvaz Jundishapur University of Medical Sciences, Ahvaz, 61357-15794, Iran.
Mikrochim Acta. 2019 Feb 1;186(3):129. doi: 10.1007/s00604-018-3217-4.
A method is described for multiple monolithic fiber solid-phase microextraction of five sterol and steroid hormones from complex food samples. A composite was prepared from graphene oxide, a metal-organic framework (ZIF-8) and a molecularly imprinted polymers was deposited on a single thin fiber. Four thin fibers were combined to obtain a fiber bundle. The nanocomposite was characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy. The parameters affecting the extraction were optimized by Box-Behnken design. Following elution with methanol, the analytes progesterone, testosterone, β-sitosterol, cholesterol and campesterol were quantified via HPLC. Response is linear in the 0.01-1000 μg L concentration range, and limits of detection range from 3 to 5 ng L. The method was successfully applied to the determination of the five analytes in spiked samples of white meat, egg yolks and vegetables. The relative mean recoveries ranged from 95.0% to 101.0%. Graphical abstract Schematic presentation of a monolith molecularly imprinting polymer (MIP) fiber fabrication for solid phase microextraction (SPME) of sterol and steroid hormones. The fiber was synthesis using graphene oxide and metal-organic framework, ZIF-8, composite by imprinting technique and progesterone as template. Four fibers were combined to obtain a fiber bundle. Then, multiple fiber solid-phase microextraction was employed for determination of analytes by coupling with HPLC/UV detection.
本文描述了一种从复杂食品样品中同时萃取五种甾体和类固醇激素的整体式纤维固相微萃取方法。将氧化石墨烯、金属有机骨架(ZIF-8)和分子印迹聚合物的复合材料沉积在单根细纤维上。将四根细纤维组合在一起,得到纤维束。通过傅里叶变换红外光谱、粉末 X 射线衍射、扫描电子显微镜(SEM)和能谱对纳米复合材料进行了表征。通过 Box-Behnken 设计优化了影响萃取的参数。用甲醇洗脱后,通过 HPLC 定量分析了孕酮、睾酮、β-谷甾醇、胆固醇和菜油甾醇。响应在 0.01-1000μg L 浓度范围内呈线性,检测限范围为 3-5ng L。该方法成功应用于测定白肉、蛋黄和蔬菜中添加的五种分析物。相对平均回收率在 95.0%至 101.0%之间。