Es'haghi Zarrin, Nezhadali Azizollah, Khatibi Aram-Dokht
Department of Chemistry, Payame Noor University, 19395-4697, Tehran, Iran.
Department of Food and Medicine, Zahedan University of Medical Sciences, 98167-43463, Zahedan, Iran.
Anal Bioanal Chem. 2016 Aug;408(20):5537-49. doi: 10.1007/s00216-016-9650-5. Epub 2016 Jun 14.
A new Fe3O4/poly(є-caprolactone) (PCL) magnetite nanocomposite was fabricated and used as a sorbent for magnetically mediated PCL microspheres solid-phase extraction (MM-PCL-SPE) followed by gas chromatography-flame ionization detection (GC-FID) for monitoring of progesterone (PGN) hormone in biological and environmental matrices, namely blood serum, tap water, urine, and hospital wastewater. The nanomagnetite core of the sorbent was synthesized by a co-precipitation method. Magnetic nanoparticles (MNPs) were then microencapsulated with PCL microspheres using emulsion polymerization. The nanocomposite was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The magnetite sorbent can be effectively dispersed in aqueous solution and attracted to an external magnetic field. The MM-PCL-SPE process for PGN assay involved (a) dispersion of the sorbent in the donor phase aqueous solution with sonication, (b) exposure to a magnetic field to collect sorbent that had adsorbed the analyte, and (c) solvent desorption of extracted PGN for GC-FID analysis. The work demonstrates the usefulness of MM-PCL-SPE in the rapid and sensitive monitoring of trace amounts of PGN in real samples. The limit of detection (LOD) and limit of quantification (LOQ) were 1.00 and 3.30 ng/mL, respectively. The relative recoveries in real samples were adequate. Linearity was observed over a wide range of 2.2-10,000.0 ng/mL in aqueous media and urine and 0.01-70.0 μg/mL in blood serum. Graphical Abstract In this research new Fe3O4/poly(є-caprolactone) (PCL) magnetite microspheres were developed as an efficient sorbent for solid-phase extraction of progesterone hormone in biological and environmental matrices.
制备了一种新型的Fe3O4/聚（ε-己内酯）（PCL）磁铁矿纳米复合材料，并将其用作吸附剂，用于磁介导的PCL微球固相萃取（MM-PCL-SPE），随后采用气相色谱-火焰离子化检测（GC-FID）来监测生物和环境基质（即血清、自来水、尿液和医院废水）中的孕酮（PGN）激素。吸附剂的纳米磁铁矿核心通过共沉淀法合成。然后使用乳液聚合法将磁性纳米颗粒（MNPs）用PCL微球微囊化。通过扫描电子显微镜（SEM）和傅里叶变换红外光谱（FTIR）对纳米复合材料进行了表征鉴定。磁铁矿吸附剂可有效分散于水溶液中，并被外部磁场吸引。用于PGN测定的MM-PCL-SPE过程包括：（a）通过超声处理将吸附剂分散于供体相水溶液中；（b）施加磁场以收集吸附了分析物吸附剂；（c）对萃取的PGN进行溶剂解吸以用于GC-FID分析。该研究证明了MM-PCL-SPE在快速灵敏监测实际样品中痕量PGN方面的实用性。检测限（LOD）和定量限（LOQ）分别为1.00和3.30 ng/mL。实际样品中的相对回收率良好。在水介质和尿液中，2.2 - 10,000.0 ng/mL的宽范围内以及血清中0.01 - 70.0 μg/mL的宽范围内均观察到线性关系。图形摘要 在本研究中，新型Fe3O4/聚（ε-己内酯）（PCL）磁铁矿微球被开发为一种高效吸附剂，用于生物和环境基质中孕酮激素的固相萃取。
