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Sensitive quantification of diphemanil methyl sulphate in human plasma by liquid chromatography–tandem mass spectrometry

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Title: Sensitive quantification of diphemanil methyl sulphate in human plasma by liquid chromatography–tandem mass spectrometry
Authors: Do, B. bernard.do@eps.ap-hop-paris.fr, Goulay-Dufaÿ, S.1, Le Hoang, M.D.1, Adoui, N.1, Graffard, H.1, Guyon, F.1, Pradeau, D.1
Source: Journal of Chromatography B: Analytical Technologies in the Biomedical & Life Sciences. Jan2007, Vol. 845 Issue 1, p104-108. 5p.
Subjects: High performance liquid chromatography, Liquid chromatography, Chromatographic analysis, Mass spectrometry, Hydrogen-ion concentration, Patient monitoring, Critical care medicine
Abstract: Abstract: A simple detection system with a high-performance liquid chromatography (HPLC) with positive ionisation-tandem mass spectrometry (ESI-MS/MS) for determining diphemanil methylsulphate (DMS) levels in human plasma using 4-diphemanylmethylene,1-methylpiperidine as an internal standard (I.S.), is proposed. The acquisition was performed with the multiple reactional monitoring (MRM) mode, by monitoring the transitions: m/z 278>262 for DMS and m/z 263>247 for the I.S. The method involved a simple single-step deproteinisation with acetonitrile. The analyte was chromatographed on a Zorbax® C18 reversed-phase chromatographic column by isocratic elution with 10−3 M ammonium acetate and 10−3 M hexafluorobutyric acid, adjusted to pH 7.0 with ammoniac/acetonitrile (40/60, v/v). The results were linear over the studied range (0.5–50.0ngmL−1) and the total analysis time for each run was 10min. The mean extraction apparent recoveries expressed at the 95% intervals of confidence were 94–104% for DMS and 92–106% for the I.S. The intra- and inter-assay precisions were 4.6–8.4% and 2.9–10.6%, respectively. The limit of quantification was 0.15ngmL−1. The devised assay was successfully applied to the residual concentrations monitoring in infant. [Copyright &y& Elsevier]
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Database: Engineering Source
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Abstract:Abstract: A simple detection system with a high-performance liquid chromatography (HPLC) with positive ionisation-tandem mass spectrometry (ESI-MS/MS) for determining diphemanil methylsulphate (DMS) levels in human plasma using 4-diphemanylmethylene,1-methylpiperidine as an internal standard (I.S.), is proposed. The acquisition was performed with the multiple reactional monitoring (MRM) mode, by monitoring the transitions: m/z 278>262 for DMS and m/z 263>247 for the I.S. The method involved a simple single-step deproteinisation with acetonitrile. The analyte was chromatographed on a Zorbax® C18 reversed-phase chromatographic column by isocratic elution with 10−3 M ammonium acetate and 10−3 M hexafluorobutyric acid, adjusted to pH 7.0 with ammoniac/acetonitrile (40/60, v/v). The results were linear over the studied range (0.5–50.0ngmL−1) and the total analysis time for each run was 10min. The mean extraction apparent recoveries expressed at the 95% intervals of confidence were 94–104% for DMS and 92–106% for the I.S. The intra- and inter-assay precisions were 4.6–8.4% and 2.9–10.6%, respectively. The limit of quantification was 0.15ngmL−1. The devised assay was successfully applied to the residual concentrations monitoring in infant. [Copyright &y& Elsevier]
ISSN:15700232
DOI:10.1016/j.jchromb.2006.07.057