Gas chromatographic mass spectrometric determination of 1,2,3-propanetrioltrinitrate (nitroglycerin) in human plasma using the nitrogen-15 labelled compound as internal standard

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Abstract
A method for the quantitative determination of 1,2,3-propanetrioltrinitrate (nitroglycerin) in human plasma by gas chromatography mass spectrometry has been developed. After addition of 1,2,3-propanetriol(15N)trinitrate as internal standard, plasma (1 ml) is extracted by a mixture of pentane and methyl acetate (90:10). The extracts are purified by partition between, first, the extraction solvent and a mixture of acetonitrile and water (60:40) and, secondly, the resultant aqueous phase and benzene. The solvent is evaporated to a small volume before injection. The fragment ions at m/z 46 and 47 are monitored for the measurement of the [NO2]+ and [15NO2]+ ions using electron impact ionization. The mean recovery (%) ±SD in blind plasma samples spiked with amounts in the concentration range 0.35-3.52 nmol I−1, was 97.4 ± 9.0 (n = 58). Within a day, recovery experiments gave rise to coefficients of variation of 9.6, 6.4 and 2.7% at the levels 0.44,0.88 and 11 nmol I−1, respectively. Concentrations in plasma down to about 0.2 nmol I−1 (50 pg mI−1) could be estimated. Percent recovery of duplicate determinations in the range 0.5-1.96 nmol I−1± SD was 99.4 ± 6.0 (n = 80).