Related substances method development and validation of an LCMS/MS method for quantification of selexipag and its related impurities in rat plasma and its application to pharmacokinetic studies

Rao, Koya Prabhakara; Babu, Namburi L. A. Amara; Koganti, Kalyani; Palakeeti, Babji; Srinivas, K.

doi:10.1007/s42452-021-04219-x

Cited by 10 publications

(10 citation statements)

References 21 publications

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“…SLP is a relatively novel active substance for the treatment of pulmonary arterial hypertension. Existing methods for determination from plasma in the literature provide assays in rat plasma (7). Human plasma analysis that provide quantitation in pharmacokinetic levels is a requirement for SLP.…”

Section: Discussionmentioning

confidence: 99%

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A novel HPLC method for selexipag in human plasma and application to a pharmacokinetic study

Ceylan

Tırıs

Tekkeli

et al. 2022

Preprint

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A novel simple and cost effective HPLC technique was presented for the quantification of selexipag (SLP) in human plasma sample and the technique's applicability to a pharmacokinetic investigation. C18 (5 µm x 4.6 mm x 150 mm) column was used at 30°C with a mobile phase consisted of acetonitrile: % 0.5 formic acid (65:35 v/v) at 1.2 mL min− 1 flow rate. The linearity range is 10–125 ng mL− 1. As sample preparation step human plasma was precipitated with acetonitrile and the detection was provided at 300 nm. LOD is found to be 3.3 ng mL− 1 for drug. Validation of the studied methods was carried out according to EMA guideline. The new method applied on a pharmacokinetic study by administration of 800 mg SLP to a healthy volunteer and parameters like AUC0 − 24, AUC0−∞, Cmax, tmax, and t1/2 were assessed.

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Section: Discussionmentioning

confidence: 99%

“…In the literature, SLP was determined by visible spectrophotometry (4), gas chromatography (5) and HPLC in bulk and pharmaceutical preparations (6). In two different studies of LC-MS/MS and UPLC-MS/MS techniques were used for determination of analyte in rat plasma (7,8).…”

Section: Introductionmentioning

confidence: 99%

A novel HPLC method for selexipag in human plasma and application to a pharmacokinetic study

Ceylan

Tırıs

Tekkeli

et al. 2022

Preprint

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“…158.63 for favipiravir (Figure 2) and m/z 602.33 ! 193.65 for remdesivir (internal standard; Figure 3) (Rao et al, 2021). The working parameters of mass spectrometry after optimization are as follows: ion spray voltage, 5500 V; temperature source, 550 C; drying gas temperature, 120-250 C; collision gas, nitrogen; pressure, 55 psi; drying gas flow stream, 5 ml/min; declustering potential, 40 V; entrance potential, 45 V; exit potential, 15 V; capillary voltage, 5,500 V; and dwell time, 1 s, respectively.…”

Section: Instrumentation and Chromatographic Conditionsmentioning

confidence: 99%

A liquid chromatography–tandem mass spectrometry method development for the quantification of favipiravir drug and its related impurities in rat plasma and its application to pharmacokinetic studies

Koganti,

Amara Babu,

Sattu

et al. 2023

Biomedical Chromatography

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Favipiravir is an antiviral drug used for the treatment of virus‐based diseases such as influenza. In this context, the development of a reliable liquid chromatography–tandem mass spectrometry method for the quantification of the drug and its impurities is necessary, particularly following the COVID‐19 pandemic. Chromatographic separation was achieved on an inertial ODS column using gradient elution with a buffer containing triethylamine in high‐performance liquid chromatography water and adjusting its pH with formic acid. The mixture of buffer and acetonitrile was used as a mobile phase with a flow rate of 1 ml/min at ambient temperature. The separation of favipiravir and its related impurities from remdesivir as an internal standard was achieved. The results indicated that all the variables, like precision, accuracy, linearity, matrix effect and stability, were successfully achieved within the limits of US Food and Drug Administration guidelines. This study could provide a new protocol for the development of new analytical methods for the detection of favipiravir and its impurities.

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“…To extract analytes from the plasma, we have employed the liquid-liquid extraction method [21][22][23]. A plasma sample of 100 µL spiked with analytes of 600 µL and IS of 500 µL was added to an Eppendorf tube of 5 mL and the mixing process has been carried out for 1 min using a vortex.…”

Section: Sample Preparationmentioning

confidence: 99%

Validation of the HPLC–PDA method for detection of eluxadoline and rifaximin in rat plasma and application in a pharmacokinetic study

et al. 2022

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Background A precise, simple, accurate, and quick HPLC–PDA method for the determination of eluxadoline and rifaximin in rat plasma was developed and validated in this study. In this method, Loperamide hydrochloride was used as the internal standard and plasma samples were prepared using a liquid–liquid extraction technique for which acetonitrile was a solvent. An Agilent Symmetry C8 column (5 µm, 250 mm × 4.6 mm) at 283 nm and isocratic elution using HPLC grade acetonitrile and 7 mM TEA (pH 2.5) with a ratio of (40: 60 v/v) was used as a mobile phase and the flow rate employed was 1 mL min−1. A satisfactory chromatographic separation was accomplished. Results An HPLC–PDA method for the determination of eluxadoline and rifaximin with retention times of 3.06 and 7.82 min, respectively, was developed. The calibration curves appear linear for both eluxadoline and rifaximin in the range of 5–200 ng mL−1 and 10–400 ng mL−1, and the corresponding correlation coefficient values were found to be 0.9999 and 0.9998 respectively. Lower limits of quantification (LLOQ) for eluxadoline and rifaximin were evaluated to be 5.0 ng mL−1 and 10.0 ng mL−1, respectively. The accuracy and precision results in all validation experiments were within the acceptance limits of FDA guidelines. Conclusion The developed HPLC–PDA approach was fully validated to meet the USFDA guidelines for bioanalytical method validation in terms of precision, accuracy, and stability. The presented approach could be beneficial for the determination of ELX and RFX in rat plasma, according to validation parameters. This is one of the efficient method to study the pharmacokinetics of ELX and RFX in rats. Graphical abstract

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Related substances method development and validation of an LCMS/MS method for quantification of selexipag and its related impurities in rat plasma and its application to pharmacokinetic studies

Cited by 10 publications

References 21 publications

A novel HPLC method for selexipag in human plasma and application to a pharmacokinetic study

A novel HPLC method for selexipag in human plasma and application to a pharmacokinetic study

A liquid chromatography–tandem mass spectrometry method development for the quantification of favipiravir drug and its related impurities in rat plasma and its application to pharmacokinetic studies

Validation of the HPLC–PDA method for detection of eluxadoline and rifaximin in rat plasma and application in a pharmacokinetic study

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