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超高效液相色谱联用石墨烯/聚苯胺纳米复合修饰电极用于磺胺类药物残留的测定

Ultra-performance liquid chromatography coupled with graphene/polyaniline nanocomposite modified electrode for the determination of sulfonamide residues.

作者信息

Thammasoontaree Nupattaranee, Rattanarat Poomrat, Ruecha Nipapan, Siangproh Weena, Rodthongkum Nadnudda, Chailapakul Orawon

机构信息

Electrochemistry and Optical Spectroscopy Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330, Thailand.

Program in Macromolecular Science, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330, Thailand.

出版信息

Talanta. 2014 Jun;123:115-21. doi: 10.1016/j.talanta.2014.02.004. Epub 2014 Feb 11.

Abstract

An ultra-performance liquid chromatography (UPLC) coupled with graphene/polyaniline (G/PANI)-modified screen-printed carbon electrode was developed for separation and sensitive determination of eight sulfonamides (SAs) in shrimp. Electrospraying was selected for electrode modification because it can generate the well dispersion of G/PANI nanocomposites on the electrode surface. Prior to electrochemical detection, eight SAs were completely separated within 7 min by using reversed phase UPLC (C4) with mobile phase containing 70:25:5 (v/v/v) of potassium hydrogen phosphate (pH 3):acetonitrile:ethanol. For amperometric detection, the detection potential acquired from hydrodynamic voltammetry was found to be +1.4V. Under optimal conditions, a wide linearity and low limit of detection were obtained for eight SAs in the range of 0.01-10 µg mL(-1) and 1.162-6.127 ng mL(-1), respectively. Compared to boron-doped diamond (BDD) electrode, a G/PANI-modified screen-printed carbon electrode offered higher sensitivity with lower operating cost. To determine SAs in shrimp samples, solid-phase extraction was used to clean up and preconcentrate the samples prior to UPLC separation. To validate this developed method, a highly quantitative agreement was accomplished with UPLC-UV system. Thus, this proposed system might be an alternative approach for rapid, inexpensive, and sensitive determination of SAs in shrimps.

摘要

开发了一种超高效液相色谱(UPLC)与石墨烯/聚苯胺(G/PANI)修饰的丝网印刷碳电极联用的方法,用于分离和灵敏测定虾中的8种磺胺类药物(SAs)。选择电喷雾法进行电极修饰,因为它能使G/PANI纳米复合材料在电极表面良好分散。在电化学检测之前,使用含有70:25:5(v/v/v)磷酸二氢钾(pH 3):乙腈:乙醇的流动相,通过反相UPLC(C4)在7分钟内将8种SAs完全分离。对于安培检测,通过流体动力学伏安法获得的检测电位为+1.4V。在最佳条件下,8种SAs的线性范围宽,检测限低,分别为0.01 - 10 μg mL(-1)和1.162 - 6.127 ng mL(-1)。与硼掺杂金刚石(BDD)电极相比,G/PANI修饰的丝网印刷碳电极具有更高的灵敏度和更低的操作成本。为了测定虾样品中的SAs,在UPLC分离之前,使用固相萃取对样品进行净化和预浓缩。为了验证所开发的方法,与UPLC - UV系统达成了高度定量的一致性。因此,该系统可能是一种快速、廉价且灵敏地测定虾中SAs的替代方法。

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