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Quantification of Piroxicam and 5'-hydroxypiroxicam in Human Plasma and Saliva Using Liquid Chromatography-Tandem Mass Spectrometry Following Oral Administration

Adriana Maria Calvo, Gabriel Mulinari Santos, Thiago José Dionísio, Maria Paula Marques, Daniel Thomas Brozoski, Vera Lúcia Lanchote, Maria Helena Raposo Fernandes, Flávio Augusto Cardoso Faria, Carlos Ferreira Santos

J Pharm Biomed Anal. 2016 Feb 20;120:212-20.

PMID: 26760238

Abstract:

Saliva sampling used to quantify piroxicam and 5'-hydroxypiroxicam is a noninvasive and painless method when compared to sequential blood sampling. For that, a rapid, selective and sensitive liquid chromatography-tandem mass spectrometric method for simultaneous determination of piroxicam and 5'-hydroxypiroxicam in saliva and human plasma was developed and validated. Piroxicam and its major metabolite were separated using a LiChroCART 125-4 RP Select-B Sorbent C18 column using a mixture of methanol and 2% phosphoric acid (pH 2.7) (70:30, v/v) for the mobile phase with a flow injection of 1mL/min. The run time was 4min. Volunteers had saliva and blood sampled before, 1, 2, 3, 4, 5, 6, 8, 11, 24, 48 and 72h after taking a 20mg oral dose of piroxicam. The pharmacokinetic parameters of piroxicam in plasma samples were as follows: AUC0-72 (64819hng/mL), predicted clearance (0.2L/h), distribution volume (14.8L), elimination half-life (50.7h) and saliva/plasma concentration ratio (0.003). The estimation of all pharmacokinetic parameters for 5'-hydroxypiroxicam would require collections beyond 72h; however, it was possible to quantify the mean maximum concentration (133ng/mL), time to peak concentration (53.6h), mean AUC0-72 (6213hng/mL), predicted clearance (110.3L/h) and saliva/plasma concentration ratio (0.04). The developed methods proved effective and sensitive for determining the lower quantification limit of piroxicam in plasma (6.1ng/mL) and saliva (0.15ng/mL) and of 5'-hydroxypiroxicam in plasma (1.2ng/mL) and saliva (0.15ng/mL).

Chemicals Related in the Paper:

Catalog Number Product Name Structure CAS Number Price
AP77459780 5′-Hydroxypiroxicam 5′-Hydroxypiroxicam 77459-78-0 Price
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