Dataset Information

Polyamines in biological samples: rapid and robust quantification by solid-phase extraction online-coupled to liquid chromatography-tandem mass spectrometry.

ABSTRACT: Polyamines are ubiquitous active biogenic amines which contribute to basic cellular functions. Hence, their quantification in samples of diverse biological origins is essential for understanding how they function, especially in disease-relevant conditions. We present here a robust, high-throughput solid-phase extraction online coupled to a liquid chromatography-tandem mass spectrometry (SPE-LC/MS/MS) approach for the simultaneous quantification of eight polyamines in various biological samples. The polyamines include 1,3-diaminopropane, putrescine, cadaverin, N-acetyl-putrescine, spermidine, spermine, N(1)-acetyl-spermine, and l-ornithine. The novelty of the work is the use of two SPE columns online coupled to LC/MS/MS, which minimizes the sample pretreatment to a single derivatization step. The analysis is complete within 4min, making the method highly suitable for routine clinical analysis and high throughput screenings. The method was fully validated with serum samples. Dynamic ranges were 0.03 to 15?g/ml for ornithine and 1 to 500ng/ml for other polyamines, which cover physiological concentrations in serum samples. Lower limits of quantification (LLoQ) were found to be between 0.1 and 5ng/ml. As a proof of concept, we investigated gender differences in polyamine levels by analyzing the serum levels of 102 subjects.

SUBMITTER: Magnes C

PROVIDER: S-EPMC3991419 | biostudies-literature | 2014 Feb

REPOSITORIES: biostudies-literature

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Polyamines in biological samples: rapid and robust quantification by solid-phase extraction online-coupled to liquid chromatography-tandem mass spectrometry.

Magnes Christoph C Fauland Alexander A Gander Edgar E Narath Sophie S Ratzer Maria M Eisenberg Tobias T Madeo Frank F Pieber Thomas T Sinner Frank F

Journal of chromatography. A 20140114

Polyamines are ubiquitous active biogenic amines which contribute to basic cellular functions. Hence, their quantification in samples of diverse biological origins is essential for understanding how they function, especially in disease-relevant conditions. We present here a robust, high-throughput solid-phase extraction online coupled to a liquid chromatography-tandem mass spectrometry (SPE-LC/MS/MS) approach for the simultaneous quantification of eight polyamines in various biological samples. ...[more]

PMID: 24485539

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Project description:It is usually a tedious task to profile the chemical composition of a given herbal medicine (HM) using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) due to the time-consuming sample preparation and laborious post-acquisition data processing procedures. Even worse, some labile compounds may face degradation risks when exposed to organic solvents for a relatively long period. As one of the most popular HMs, the promising therapeutic benefits of Epimedii Herba (Chinese name: Yinyanghuo) are well defined; however, the chemical profile, and in particular those flavonoids that have been claimed to be responsible for the efficacy, remains largely unknown. Attempts are devoted here to achieve direct LC-MS measurement and efficient post-acquisition data processing, and chemome comparison among three original sources of Epimedii Herba, such as Epimedium sagittatum (Esa), E. pubescens (Epu), and E. koreanum (Eko) was employed to illustrate the strategy utility. A home-made online liquid extraction (OLE) module was introduced at the front of the analytical column to comprehensively transfer the compounds from raw materials onto the LC-MS instrument. A mass defect filtering approach was programmed to efficiently mine the massive LC-MS dataset after which a miniature database was built involving all chemical information of flavonoids from the genus Epimedium to draw a pentagonal frame to rapidly capture potential quasi-molecular ions (mainly [M-H]-). A total of 99 flavonoids (66 in Esa, 84 in Eko, and 66 in Epu) were captured, and structurally annotated by summarizing the mass fragmentation pathways from the mass spectrometric data of authentic compounds and an in-house data library as well. Noteworthily, neutral loss of 144 Da was firstly assigned to the neutral cleavage of rhamnosyl residues. Significant species-differences didn't occur among their chemical patterns. The current study proposed a robust strategy enabling rapid chemical profiling of, but not limited to, HMs.

Dataset Information

Polyamines in biological samples: rapid and robust quantification by solid-phase extraction online-coupled to liquid chromatography-tandem mass spectrometry.

Publications

Polyamines in biological samples: rapid and robust quantification by solid-phase extraction online-coupled to liquid chromatography-tandem mass spectrometry.

Similar Datasets

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