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 s
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 s
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稳定同位素标记衍生化结合磁分散固相萃取通过体内微透析和超高效液相色谱串联质谱测定含羟基胆固醇及其代谢物
DOI：
10.1016/j.chroma.2019.02.021
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发表时间：
2019-06
影响因子：
4.1
通讯作者：
Wang Xiao
中科院分区：
文献类型：
--
作者：
Wang Xin;Sun Jing;Zhao Xian En;Xu Yanqiu;Sun Luping;Zhu Shuyun;You Jinmao;Wang Xiao
含羟基的胆固醇和代谢物（HCM）是阿尔茨海默病的潜在生物标志物。因此，HCM的定量分析可以作为临床诊断和药物治疗的指标。在这项工作中，我们开发了一种准确、灵敏、快速的方法，通过微波辅助稳定同位素标记衍生化（MA-SILD）磁分散固相萃取（MDSPE）结合超高效液相色谱电喷雾电离串联质谱（UHPLC-ESI-MS/MS）在多反应监测模式（MRM）下测定大鼠血液微透析液中的HCM。在这方面，设计、合成了一对新的SILD试剂，d0-/d3-3-N-甲基-2'-羧基罗丹明6G（d0-/d3-MCR6G），并用于标记HCM。将具有永久正电荷的罗丹明 6G 引入 HCM 中，提高了电离效率并增强了检测灵敏度。此外，d3-MCR6G标记标准品作为内标，减少了基质效应，保证了准确的定量。对影响 MA-SILD 和 MDSPE 的各种因素进行了优化。此外，在 2–3000pg/mL 的浓度范围内，获得了良好的线性，R2> 0.994。检测限 (LOD) 和定量限 (LOQ) 分别在 0.24–0.31 和 1.5–1.8pg/mL 范围内。达到了可接受的精密度（1.6-12.6%）、准确度（87.9-105.2%）、基质效应（85.4-111.2%）和衍生化效率（>98%）。总体而言，该方法经过验证，可用于大鼠血液微透析液中 HCM 的准确、灵敏且简单的定量。该工作将为AD或其他神经系统疾病的诊断和治疗提供一定的技术支持。
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, thed3-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 limits of detection (LODs) and quantitation (LOQs) were in the range of 0.24–0.31 and 1.5–1.8 pg/mL, respectively. Acceptable precision (1.6–12.6%), accuracy (87.9–105.2%), matrix effect (85.4–111.2%) and derivatization efficiency (>98%) were achieved. On the whole, this method was validated and applied to accurate, sensitive and simple quantitation of HCMs in rat blood microdialysates. This work would provide some technical support in the diagnosis and treatment of AD or other neurological diseases.
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影响因子：
7.2
作者：
Selkoe, Dennis J.
通讯作者：
Selkoe, Dennis J.
影响因子：
6.1
作者：
Alinezha, Heshmatollah;Amiri, Amirhassan;Maleki, Behrooz
通讯作者：
Maleki, Behrooz
影响因子：
168.9
作者：
Ballard, Clive;Gauthier, Serge;Jones, Emma
通讯作者：
Jones, Emma
DOI：
10.1016/j.chroma.2016.05.071
发表时间：
2016-07
期刊：
Journal of chromatography. A
影响因子：
--
作者：
Jianrong Wu;Hongyan Zhao;Deli Xiao;P. Chuong;Jia He;Hua He
通讯作者：
Jianrong Wu;Hongyan Zhao;Deli Xiao;P. Chuong;Jia He;Hua He
DOI：
10.1016/j.chroma.2017.01.039
发表时间：
2017-03
期刊：
Journal of chromatography. A
影响因子：
--
作者：
Petri Kylli;T. Hankemeier;R. Kostiainen
通讯作者：
Petri Kylli;T. Hankemeier;R. Kostiainen