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2 Acta Chromatographica

2 2016

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Fast and Sensitive RP-HPLC—Fluorescence Method for the Quantitative Analysis of Moxifloxacin in Rat Plasma and Its Application to a Preclinical Pharmacokinetic Study

Hurtado F. K., Kaiser M., Tasso L., Costa T.

Acta Chromatographica

2016

Vol. 28, no. 2

175--191

A fast, simple, and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and fully validated for the determination of moxifloxacin (MXF) in rat plasma. MXF and gatifloxacin (internal standard, I.S.) were extracted from plasma by single-step protein precipitation with acidified acetonitrile. Chromatographic separation was accomplished in less than 8 min on an Atlantis ® T3 column with 0.4% aqueous triethylamine–methanol–acetonitrile (60:35:5, v/v/v) solution as mobile phase. Detection was achieved by fluorescence (λexcitation = 295 nm, λemission = 500 nm), and the calibration curves were found to be linear over the plasma concentration range of 10–2,500 ng mL−1 with a mean correlation coefficient (r) of 0.9946 (n = 6). The intra- and inter-assay imprecision (% CV) was less than 2.4 and 3.3%, respectively, and the accuracy was >90%. The mean extraction recoveries for MXF and I.S. from plasma were 77 and 82%, respectively. The method was also validated for specificity, sensitivity, and stability; all the results were within the acceptable range. The proposed method was then successfully applied to the quantitative analysis of MXF in rat plasma samples, being a valuable and high-throughput assay to support ongoing pharmacokinetic studies on this promising anti-infective agent.

Development and validation of a sensitive and selective LC—MS/MS method for the determination of an antimalarial drug candidate in rat plasma, and its application to a preclinical pharmacokinetic study

Pires C., Kaiser M., Grünspan L. D., Barreto F., Innocente A., Gnoatto S., Laureano J. V., Araujo B., Costa T., Tasso L.

Acta Chromatographica

2016

Vol. 28, no. 4

439--453

An accurate and reliable LC—MS/MS assay was firstly developed and validated for quantitative determination of a new antimalarial prototype drug, 3β-hydroxyurs-12-en-28-oic acid (LAFIS 01), in rat plasma. Dexamethasone was employed as internal standard. Simple protein precipitation by acetonitrile for the sample preparation was used. Effective separation was achieved with Phenomenex Luna C18 (50 × 2 mm, 5 μm) column. The mobile phase consisted of (A) water and (B) acetonitrile, both containing 0.1% acetic acid, delivered by gradient elution. The column temperature was maintained at 40 °C. The LAFIS 01 was monitored by electrospray ionization interface, operating in the negative mode (ESI−) in multiple reactions monitoring (MRM), checking the transitions 455 > 455 for LAFIS 01 and 451 > 361 for the IS. Once LAFIS 01 demonstrated low fragmentation by collision-induced dissociation (CID) nonpresenting abundant high-intensity fragments to meet the desired concentration levels quantification, only pseudomolecular ion was monitored. The flow rate was 500 μL min−1. The lower limit of quantitation achieved was 10 ng mL−1 and linearity was observed from 10 to 500 ng mL−1. The relative standard deviation (RSD) values of the intra- and inter-assay precisions of the method were below 8.42 and 7.94%, respectively. The accuracy ranged from 92.05 to 102.94%. The extraction recovery of LAFIS 01 and IS was up to 90%. The method showed linearity, precision, accuracy, sensitivity, and stability required to quantify LAFIS 01 in preclinical pharmacokinetic study.