Stable isotope labeling derivatization coupled with magnetic dispersive solid phase extraction for the determination of hydroxyl-containing cholesterol and metabolites by in vivo microdialysis and ultra-high performance liquid chromatography tandem mass spectrometry

Journal of Chromatography. a
Xin WangXiao Wang

Abstract

Hydroxyl-containing cholesterol and metabolites (HCMs) are potential biomarkers for Alzheimer's disease. Therefore, quantitative analysis of HCMs can serve as an indicator of clinical diagnosis and drug treatment. In this work, we developed an accurate, sensitive and rapid method for the determination of HCMs in rat blood microdialysates by microwave-assisted stable isotope labeling derivatization (MA-SILD) magnetic dispersive solid phase extraction (MDSPE) coupled with ultra-high performance liquid chromatography electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS) in the multiple reaction monitoring mode (MRM). In this respect, a pair of new SILD reagents, d0-/d3-3-N-methyl-2'-carboxyl Rhodamine 6G (d0-/d3-MCR6G), were designed, synthesized and used to label HCMs. Rhodamine 6G with permanently positive charge was introduced into HCMs, improving ionization efficiency and enhancing detection sensitivity. In addition, the d3-MCR6G labeled standards were served as internal standards, reducing the matrix effect and guaranteeing accurate quantification. Various factors affecting MA-SILD and MDSPE were optimized. Furthermore, good linearity was obtained with R2 > 0.994 over the concentration range of 2-3000 pg/mL. The ...Continue Reading

Citations

Jan 17, 2020·Journal of Separation Science·Qiong JiangMin Sun
Dec 11, 2019·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Qiong JiangMin Sun

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