In‐tube solid‐phase microextraction (sulfopropyl methacrylate‐co‐ethylene glycol dimethacrylate monolithic capillary) coupled to LC–MS/MS to determine beta amyloid peptides in Alzheimer's cerebrospinal fluid samples

IF 1.3 Q4 CHEMISTRY, ANALYTICAL SEPARATION SCIENCE PLUS Pub Date : 2023-08-07 DOI:10.1002/sscp.202300044
Caroline Fernandes Grecco, V. Tumas, J. Hallak, M. E. Queiroz
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Abstract

Alzheimer's disease (AD) is a neurodegenerative disorder characterized by an extracellular accumulation of amyloid beta peptides in the brain. The concentration of the amyloid beta peptides in cerebrospinal fluid (CSF) have been evaluated as potential biomarkers of AD for early diagnostic. In this work, an in‐tube solid‐phase microextraction (in‐tube SPME) coupled to UHPLC–MS/MS method was established to determine amyloid beta peptides in CSF samples from AD patients. A strong cation‐exchange (sulfopropyl methacrylate‐co‐ethylene glycol dimethacrylate) monolithic capillary was synthesized on the inner surface of a fused silica capillary and used as an extractive phase for in‐tube SPME. The morphology and chemical structure of the monolithic phase were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The proposed method presented linear range from the lower limits of quantification 0.6 and 0.8 to 10 ng mL−1. Excluding the lower limits of quantification values, the analytical validation showed precision with the coefficient of variation values lower than 13.1%, and accuracy with relative standard deviation lower than 13.5%. The in‐tube SPME coupled to UHPLC–MS/MS method was successfully applied to determine amyloid beta peptides in CSF samples from AD patients.
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管内固相微萃取(甲基丙烯酸磺丙酯-乙二醇二甲基丙烯酸酯整体毛细管)与LC–MS/MS联用测定阿尔茨海默氏症脑脊液样本中的β-淀粉样肽
阿尔茨海默病(AD)是一种神经退行性疾病,其特征是大脑中淀粉样β肽的细胞外积聚。脑脊液(CSF)中淀粉样蛋白β肽的浓度已被评估为AD早期诊断的潜在生物标志物。在这项工作中,建立了一种管内固相微萃取(管内SPME)与UHPLC–MS/MS相结合的方法来测定AD患者CSF样本中的淀粉样蛋白β肽。在熔融石英毛细管的内表面合成了一种强阳离子交换(甲基丙烯酸磺丙酯-乙二醇二甲基丙烯酸酯)整体毛细管,并用作管内SPME的萃取相。利用扫描电子显微镜和傅立叶变换红外光谱对单体相的形貌和化学结构进行了表征。所提出的方法呈现出从定量下限0.6和0.8到10 ng/mL−1的线性范围。除去定量值的下限,分析验证显示,变异系数值的准确度低于13.1%,相对标准偏差的准确度小于13.5%。管内SPME与UHPLC–MS/MS相结合的方法成功应用于AD患者CSF样品中淀粉样β肽的测定。
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来源期刊
SEPARATION SCIENCE PLUS
SEPARATION SCIENCE PLUS CHEMISTRY, ANALYTICAL-
CiteScore
1.90
自引率
9.10%
发文量
111
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