Ma Jian-Bo, Qiu Hai-Wen, Rui Qiu-Hong, Liao Yu-Feng, Chen Yan-Min, Xu Jin, Zhan Ping-Ping, Zhao Yong-Gang
Ningbo No.2 Hospital, Ningbo, Zhejiang 315010, China.
Ningbo First Hospital, Ningbo, Zhejiang 315010, China.
J Chromatogr A. 2016 Jan 15;1429:86-96. doi: 10.1016/j.chroma.2015.12.030. Epub 2015 Dec 14.
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.
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。