title: Facile synthesis of a boronate affinity sorbent from mesoporous nanomagnetic polyhedral oligomeric silsesquioxanes composite and its application for enrichment of catecholamines in human urine.
abstract: A boronate-decorated nanomagnetic organic-inorganic hybrid material was facilely synthesized by utilizing the nanomagnetic polyhedral oligomeric silsesquioxanes (POSS) composite (Fe3O4@POSS) as the base platform. A simple copolymerization occurred between 3-acrylamidophenylboronic acid (AAPBA) and the residual end vinyl groups supplied by the substrate. Here the special emphasis was placed on the octavinyl POSS, which not only acted as the building blocks for a hybrid architecture but also facilitated the process of grafting boronate groups onto the surface of POSS based nanomagnetic composite (Fe3O4@POSS). The successful immobilization of affinity ligand-AAPBA on the Fe3O4@POSS was confirmed by Fourier transform infrared (FT-IR), elemental analysis, inductively coupled plasma atomic emission spectrometer (ICP-AES), field emission scanning electron microscope. A magnetic solid-phase extraction (MSPE) for cis-diols enrichment was developed using the as-prepared Fe3O4@POSS-AAPBA material as an affinity sorbent and three catecholamines (CAs), namely noradrenaline, epinephrine and isoprenaline, as model analytes. Under the optimal extraction conditions, sensitive and simultaneous analysis of three CAs from the urine sample was achieved by high-performance liquid chromatography with UV detection (HPLC-UV). The limits of detection (LOD, S/N = 3) and the limits of quantitation (LOQ, S/N = 10) for the target analytes were 0.81-1.32 ng mL-1and 2.70-4.40 ng mL-1, respectively. Also good recoveries (85.5-101.7%) and repeatability (RSD≤10.1%) were obtained by this method. This work not only showed a facility for the utilization of Fe3O4@POSS as a substrate for constructing a boronate functionalized nanomagnetic sorbent, but also demonstrated the capability of the derived material for recognition of trace amount of cis-diols biomolecules presented in complicated biological matrices.
authors: Department of Chemistry, Shanghai University, Shanghai 200444, PR China; Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China. Electronic address: hbhe2006@shu.edu.cn.
authors: Haibo
authors: H
authors: He
authors: Department of Chemistry, Shanghai University, Shanghai 200444, PR China.
authors: Ziqing
authors: Z
authors: Zhou
authors: Department of Chemistry, Shanghai University, Shanghai 200444, PR China.
authors: Chen
authors: C
authors: Dong
authors: Department of Chemistry, Shanghai University, Shanghai 200444, PR China.
authors: Xin
authors: X
authors: Wang
authors: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors: Qiong-Wei
authors: QW
authors: Yu
authors: Department of Chemistry, Shanghai University, Shanghai 200444, PR China.
authors: Yunyi
authors: Y
authors: Lei
authors: Department of Chemistry, Shanghai University, Shanghai 200444, PR China.
authors: Liqiang
authors: L
authors: Luo
authors: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors: Yuqi
authors: Y
authors: Feng
mesh_terms: D000327:Adsorption; D001897:Boronic Acids / Q000737:chemistry*; D002395:Catecholamines / Q000737:chemistry / Q000652:urine*; D060326:Chemistry Techniques, Synthetic; D006801:Humans; D006863:Hydrogen-Ion Concentration; D058185:Magnetite Nanoparticles / Q000737:chemistry*; D017646:Organosilicon Compounds / Q000138:chemical synthesis* / Q000737:chemistry*; D058105:Polymerization; D016062:Porosity; D012997:Solvents / Q000737:chemistry; D013997:Time Factors; D016482:Urinalysis / Q000379:methods*
chemical_list: C419826:3-acrylamidophenylboronic acid; D001897:Boronic Acids; D002395:Catecholamines; D058185:Magnetite Nanoparticles; D017646:Organosilicon Compounds; D012997:Solvents
keywords: Boronate affinity material; CAs; Fe(3)O(4)@POSS; Magnetic solid-phase extraction; Urine samples