Electrospray-Mass Spectrometric Analysis of Plasma Pyrophosphates Separated on a Multi-Modal Liquid Chromatographic Column

Title
Electrospray-Mass Spectrometric Analysis of Plasma Pyrophosphates Separated on a Multi-Modal Liquid Chromatographic Column
Authors
이수현이정애이원용정봉철최만호
Keywords
Pyrophosphate; Isoprenoids; LC-MS; Multi-modal column; Statins; Cardiovascular disease
Issue Date
2011-12
Publisher
Mass Spectrometry Letters
Citation
VOL 2, NO 4, 92-95
Abstract
Pyrophosphates are the key intermediates in the biosynthesis of isoprenoids, and their concentrations could reveal the benefits of statins in cardiovascular diseases. Quantitative analysis of five pyrophosphates, including isopentenyl pyrophosphate (IPP), dimethylallyl pyrophosphate (DMAPP), geranyl pyrophosphate (GPP), farnesyl pyrophosphate (FPP), and geranylgeranyl pyrophosphate (GGPP), was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative ionization mode. After dilution with methanol, samples were separated on a 3 μm particle multi-modal C18 column (50 × 2 mm) and quantified within 10 min. The gradient elution consists of 10 mM ammonium bicarbonate and 0.5% triethylamine (TEA) in water and 0.1% TEA in 80% acetonitrile was used at the flow rate of 0.4 mL/min. Overall recoveries were 51.4-106.6%, while the limit of quantification was 0.05 μg/mL for GPP and FPP and 0.1 μg/mL for IPP, DMAPP, and GGPP. The precision (% CV) and accuracy (% bias) of the assay were 1.9-12.3% and 89.6-111.8%, respectively, in 0.05-10 μg/mL calibration ranges (R2 > 0.993). The devised LC-MS/MS technique with the multi-modal C18 column can be used to estimate the biological activity of pyrophosphates in plasma and may be applicable to cardiovascular events with cholesterol metabolism as well as the drug efficacy of statins.
URI
http://pubs.kist.re.kr/handle/201004/41427
ISSN
2093-8950
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KIST Publication > Article
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