Validation of an LC–MS/MS method for quantitation of fostemsavir in plasma

A linear and accurate liquid chromatographic tandem mass spectrometric (LC-MS/MS) technique for the quantitation of capmatinib in plasma was developed and subjected for validation. Canagliflogin was employed as an internal standard (IS). Extraction of plasma was executed utilizing 5 mL of ethyl acetate solvent. Analysis was performed Zorbax ODS (50 mm × 2.1 mm x 3 μ) stationary phase at room conditions and a movable solvent composition of 0.1% HCOOH, acetonitrile and methyl alcohol (15:50:35). The flowing rate of the movable phase was 0.4 mL/min. Drug and IS were identified in positive mode of ionization with electrospray mode to get the mass transitions of (m/z): Capmatinib, 413.15/386.14 and canagliflogin (IS), 445.15/267.12. The correlation between capmatinib concentrations and their respective peak proportions to canagliflogin was a straight line over 0.2 to 3200 ng/mL concentration levels. Intra day and inter-day precisions were ≤5.18% for capmatinib. Inter and intra day bias were within the range of −4.17 to 4.53%. The mean measured extraction recovery of capmatinib was 99.23%. Recovery of IS was 98.31%. Capmatinib was subjected for long-term, freeze thaw, bench top, short-term stability, auto-sampler, dry extract, and stock solution stability at low QC and high QC levels and it was stable at all these conditions. The established technique can be utilized to regularly quantitfy of capmatinib in plasma samples in industries, forensic labs, and clinical research organizations.

“…Specificity, accuracy, linearity, precision, stability, and recovery were among the validation criteria. [12][13][14][15][16][17][18][19]…”

Section: Validation Of the Analytical Methodsmentioning

confidence: 99%

“…Figure 2B shows blank plasma that has been spiked with the IS at a concentration of 750 ng/mL. [15][16][17][18]…”

Section: Specificitymentioning

confidence: 99%

Stability Indicating an LC-MS/MS Method Development and Validation for the Quantification of Capmatinib in Human Plasma

Panigrahi

2023

“…The appropriateness of the system was examined on a daily basis during the method validation. [12][13][14][15] The results showed that the analyte and ISTD both had retention times with %CV values less than 0.28. The coefficient of variation of the peak area ratio (Analyte area/ ISTD area) was less than 0.18% CV.…”

Section: System Suitabilitymentioning

confidence: 98%

“…When comparing extracted and un-extracted plasma quality control solutions at MQC, HQC, and LQC concentrations 13 , the average recoveries in percent were determined. Mean recoveries for Futibatinib were from 98.49 to 99.35 percent at MQC, 99.35 to 98.47%vat HQC, and 98.47% at LQC.…”

Section: Recoverymentioning

confidence: 99%

Development of Stability Indicating Method for the Quantification of Futibatinib in K2EDTA Human Plasma by LC-MS/MS

Jogeswararao,

Bhikshapathi

2023

sensitive, accurate, and linear LC-MS/MS method for the quantification of futibatinib in human plasma K2 ethylene diamine tetraacetic acid (EDTA) was developed. A Phenomenex C18, 150×4.60 mm, 2.1 μ column, 0.1% HCCOH, ACN and methyl alcohol (13/67/20, v/v/v) mobile solvent system at 0.8 mL/min was employed for the isolation of components.10 μL. of volumes were employed to isolate the peak responsess within 2.0 minutes at 40 ± 5ºC of oven temperature. Analyte retention was 1.261 minutes and ISTD of 1.292 minutes. Throughout the process of validation, each of the four calibration curves exhibited linear behavior for standards with concentrations ranging from 0.16 to 3250 ng/mL. Validation showed an r2 = 0.9997. At MQC, HQC, and LQC concentrations, futibatinib had 98.49, 99.35, and 98.47% mean recovery. Every QC level had a mean recovery of 90.51% and a %CV of 3.06. All of the control solutions had back-calculated concentration values that were accurate between 94.61 and 98.86% of the time. The range of %CV of back-calculated values for all quality control samples were in the range of 0.6 and 4.63, which is within the acceptable range of 15%. The developed method can be applied successfully for the quantification of the Futibatinib in biological matrices.

“…Two blank plasma samples were derived from 8 different screened plasma batches, which included one lipemic and one hemolytic plasma batch. [18][19][20] Each replication was treated separately. One set of eight distinct blank matrices was used to introduce the LQC concentration and the internal standard (ISTD).…”

Section: Matrix Effectmentioning

confidence: 99%

An LC-MS Method Development and Validation for the Estimation of Ritonavir in Plasma Samples

Katthala,

Gubbiyappa

2024

This project aims to create and verify a method using high-performance liquid chromatography-mass spectrometry (HPLC-MS) to measure the amount of ritonavir in human plasma. Saquinavir will be used as the internal standard for this analysis. Chromatographic isolation was processed HYPURITY ADVACE 50 × 4.6 mm, 5 μm (Make: Thermo scientific) analytical column with mobile phase composition of methanol and ammonium acetate 5 mm buffer in the ratio of 85:15% v/v. Detection was processed in a positive ionic approach and the parent and product ion transitions were monitored at 721.30/296.10 for ritonavir and 671.30/570.30 for saquinavir (API 2000). The measurement of the linearity curve for regression analysis The correlation coefficient (r) exhibited a remarkable value of over 0.99 within the concentration range of 8.004 to 1600.001 ng/mL for ritonavir. All eight batches showed no significant matrix effect. It was found that the standardized matrix factor had a precision of 1.90% at the LQC level and 2.38% at the HQC level. It was 0.992 for LQC and 1.005 for HQC when the IS factor was taken into account. Ritonavir had a general recovery rate of 89.07%, with a range of accuracy from 0.85 to 2.55%. The internal standard drug saquinavir had an average recovery rate of 90.18%, with a range of accuracy from 1.89 to 3.40%. The developed method was successfully validated and can be utilized for the assessment of ritonavir in biological matrices in industries, forensic labs, quality control labs, and bioavailability studies.