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Study on the drug–drug interaction of antituberculosis drugs — PA-824 and moxifloxacin based on pharmacokinetics in rats by LC–MS/MS

Jing Juan, Jia Yuting, Feng Tian, Xie Tian, Li Zhoupeng, Hao Yong, Wang Libin

Acta Chromatographica

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2019

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Vol. 31, no. 3

206--210

EN

A simple, rapid, and sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous quantitation of PA-824 and moxifloxacin in rat plasma using carbamazepine as an internal standard (IS). The sample preparation involved a one-step protein precipitation method with methanol. The separation was performed on Inertsil® ODS3 C18 column (150 mm × 4.6 mm, 5 μm) and maintained at 30 °C. The mobile phase consisted of 0.1% formic acid in acetonitrile–water (90:10 v/v) with fast isocratic elution at a flow rate of 0.6 mL/min and a run time of 10 min. A mass spectrometer was run in the positive ion electrospray ionization (ESI) mode using multiple reaction monitoring (MRM) to monitor the mass transitions. The MRM transitions were chosen to be m/z 360.1 → m/z 175.0 for PA-824, m/z 402.0 → m/z 383.9 for moxifloxacin, and m/z 237.1 → m/z 194.0 for IS. The method was fully validated in terms of selectivity, linearity, accuracy, precision, matrix effect, recovery, and stability, respectively. The method was successfully applied to drug–drug interaction (DDI) study of PA-824 and moxifloxacin in rats. The results show that the main pharmacokinetic parameters of PA-824, namely, Tmax, t1/2, and AUC(0–t), increased more in the PA-824 and moxifloxacin group than in the PA-824 group. However, there were little changes in the main pharmacokinetic parameters of moxifloxacin from single and combined groups.

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An HPLC method for the determination of moxifloxacin in breast milk by fluorimetric detection with precolumn derivatization

Tekkeli S. E., Gazioglu I., Kiziltas M. V.

Acta Chromatographica

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2017

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Vol. 29, no. 1

57--65

EN

A new, sensitive, and selective high-performance liquid chromatography (HPLC) method with fluorimetric detection was developed for the determination of moxifloxacin (MOX) in human breast milk. MOX was precolumn derivatized with fluorescamine; the fluorescent derivative was separated on an RP C18 column using a mobile phase composed of acetonitrile–10 mM orthophosphoric acid by isocratic elution with flow rate of 0.5 mL min -1. The method was based on the measurement of the derivative using fluorescence detection at 481 nm with excitation at 351 nm. The calibration curve was linear over the range of 1–40 μg Ml -1. Limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.3 and 1 μg Ml -1, respectively. Intra-day and interday repeatabilities were less than 3.15%.

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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

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2016

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Vol. 28, no. 2

175--191

EN

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.