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采用羧基功能化磁性碳纳米管分子印迹聚合物结合液相色谱-串联四极杆质谱法快速测定人血浆中的儿茶酚胺。

Fast determination of catecholamines in human plasma using carboxyl-functionalized magnetic-carbon nanotube molecularly imprinted polymer followed by liquid chromatography-tandem quadrupole mass spectrometry.

作者信息

Ma Jian-Bo, Qiu Hai-Wen, Rui Qiu-Hong, Liao Yu-Feng, Chen Yan-Min, Xu Jin, Zhan Ping-Ping, Zhao Yong-Gang

机构信息

Ningbo No.2 Hospital, Ningbo, Zhejiang 315010, China.

Ningbo First Hospital, Ningbo, Zhejiang 315010, China.

出版信息

J Chromatogr A. 2016 Jan 15;1429:86-96. doi: 10.1016/j.chroma.2015.12.030. Epub 2015 Dec 14.

Abstract

A novel, simple and sensitive method based on the use of dispersive micro-solid-phase extraction (d-μ-SPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) for the determination of catecholamines, i.e., dopamine (DA), norepinephrine(NE) and epinephrine (E), was developed and validated. The novel catecholamines molecularly imprinted polymer (MIP) on the surface of carboxyl-functionalized magnetic-carbon nanotube (CF@m-CNTs-MIP) was synthesized and characterized by vibrating sample magnetometer (VSM), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The CF@m-CNTs-MIP was used as the d-μ-SPE sorbent to extract catecholamines from human plasma samples. The obtained results demonstrated the higher extraction capacity of CF@m-CNTs-MIP with recoveries between 87.5-110%. The limits of quantification (LOQs) for NE, E and DA were 76 ng/L, 18 ng/L and 10 ng/L, respectively. Validation results on linearity, specificity, accuracy, precision and stability, as well as on application to the analysis of catecholamines in 120 healthy volunteers demonstrated the applicability to clinical studies.

摘要

建立并验证了一种基于分散微固相萃取(d-μ-SPE)结合超快速液相色谱-串联四极杆质谱(UFLC-MS/MS)的新颖、简单且灵敏的方法,用于测定儿茶酚胺,即多巴胺(DA)、去甲肾上腺素(NE)和肾上腺素(E)。合成了羧基功能化磁性碳纳米管(CF@m-CNTs-MIP)表面的新型儿茶酚胺分子印迹聚合物(MIP),并通过振动样品磁强计(VSM)、扫描电子显微镜(SEM)和X射线光电子能谱(XPS)对其进行了表征。CF@m-CNTs-MIP用作d-μ-SPE吸附剂,从人血浆样品中提取儿茶酚胺。所得结果表明CF@m-CNTs-MIP具有较高的萃取能力,回收率在87.5%-110%之间。NE、E和DA的定量限(LOQ)分别为76 ng/L、18 ng/L和10 ng/L。线性、特异性、准确性、精密度和稳定性的验证结果,以及在120名健康志愿者中儿茶酚胺分析的应用结果,证明了该方法在临床研究中的适用性。

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