Application of isotope-based carboxy group derivatization in LC–MS/MS analysis of tissue free-fatty acids for thyroid carcinoma

Workflow for the FFAs analysis in tissue samples based on DMPP derivatization. •A MS-based analytical strategy for tissue FFAs was successfully established by isotope labeling.•The entire method was carried out under mild conditions with high sensitivity and specificity.•The optimized workflow was b...

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Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 2013-10, Vol.84, p.256-262
Main Authors: Leng, Jiapeng, Guan, Qing, Sun, Tuanqi, Wu, Yi, Cao, Yanjing, Guo, Yinlong
Format: Article
Language:English
Subjects:
acids
Carboxylic Acids - chemistry
carcinoma
Chromatography, Liquid - methods
Derivatization
Dimethylphenylpiperazinium Iodide - chemistry
fatty acid metabolism
Fatty Acids, Nonesterified - analysis
Fatty Acids, Nonesterified - chemistry
Free fatty acid
free fatty acids
Humans
Isotope labeling
Isotope Labeling - methods
Isotopes - chemistry
LC–MS/MS
Lipid Metabolism
lipids
Lipids - chemistry
monitoring
patients
Sensitivity and Specificity
system optimization
Tandem Mass Spectrometry - methods
Thyroid carcinoma
Thyroid Neoplasms - chemistry
Thyroid Neoplasms - metabolism
tissue analysis
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Summary:Workflow for the FFAs analysis in tissue samples based on DMPP derivatization. •A MS-based analytical strategy for tissue FFAs was successfully established by isotope labeling.•The entire method was carried out under mild conditions with high sensitivity and specificity.•The optimized workflow was build up for the practical and convenient FFAs assay.•Enhanced accuracy in quantitation was achieved by the introduction of isotopic internal standard. Free fatty acids (FFAs) analysis of human tissue is challenging due to the low abundance of tissue lipids and interference from the complex matrix. Based on our previously reported on 2,4-dimethoxy-6-piperazin-1-yl pyrimidine (DMPP) derivatization toward carboxy group, we have further applied DMPP derivatization method in the assay of tissue FFAs in patients with thyroid carcinoma after method optimization including sample pretreatment, and derivatization condition. d6-DMPP labeled mixture of FFAs standard was used as the internal standard (IS). The d0-DMPP labeled samples (spiked with IS) were subsequently used for lipids profiling by selective reaction monitoring (SRM) detection. The DMPP derivatization combined with SRM not only allowed trace analysis of FFAs in complex matrix due to the extremely high sensitivity, but also minimized the errors in quantitation because of the very similar property between d0-DMPP derivatized samples and d6-DMPP derivatized IS. Eighteen kinds of FFAs were detected successfully with the increased level in carcinoma tissue compared with the normal tissue, which may be the results of abnormality in the metabolism of fatty acid synthases and lipids. Application of the DMPP based FFAs derivatization is expected to provide a promising tool for the investigation of lipids in vivo, especially for the research of lipid metabolism.
ISSN:0731-7085
1873-264X
DOI:10.1016/j.jpba.2013.06.004