Liquid chromatography tandem mass spectrometry method for the estimation of lamotrigine in human plasma: Application to a pharmacokinetic study

Abstract

A reliable, selective and sensitive liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of lamotrigine in human plasma using lamotrigine-13C3, d3 as an internal standard. Analyte and internal standard were extracted from human plasma by solid-phase extraction and detected in positive ion mode by tandem mass spectrometry with electrospray ionization (ESI) interface. Chromatographic separation was performed on a Chromolith® SpeedROD; RP-18e column (50−4.6 mm i.d.) using acetonitrile: 5±0.1 mM ammonium formate solution (90:10, v/v) as the mobile phase at a flow rate of 0.500 mL/min. The calibration curves were linear over the range of 5.02–1226.47 ng/mL with the lower limit of quantitation validated at 5.02 ng/mL. The analytes were found stable in human plasma through three freeze (−20 °C)-thaw (ice-cold water bath) cycles and under storage on bench-top in ice-cold water bath for at least 6.8 h, and also in the mobile phase at 10 °C for at least 57 h. The method has shown good reproducibility, as the intra- and inter-day precisions were within 3.0%, while the accuracies were within ±6.0% of nominal values. The validated LC–MS/MS method was applied for the evaluation of pharmacokinetic and bioequivalence parameters of lamotrigine after an oral administration of 50 mg lamotrigine tablet to thirty-two healthy adult male volunteers.

Method Development and Validation for Measuring O6-Methylguanine in Dried Blood Spot Using Ultra High-Performance Liquid Chromatography Tandem Mass Spectrometry

“…The calibration curve obtained was linear and meets the requirements of the correlation coefficient (r) value greater than 0.98. 15 The results of the calibration curve experiment showed that the %diff obtained fulfilled the requirements. Data of O 6 -methylguanine inter-day calibration curves are shown in Table 4 .…”

Development and validation of doxorubicin hydrochloride and doxorubicinol quantification method in dried blood spot by liquid chromatography–tandem mass spectrometry

“…Calibration standards were prepared and analyzed by plotting the peak area ratios of the analyte to the internal standard versus the nominal concentration in triplicate. Calibration curves were considered acceptable when the correlation coefficient ( r ) was greater than 0.98 for biological matrix,[ 14 ] and the bias of the calculated concentrations was within ±15% of the nominal concentrations, except the LLOQ with an allowed deviation of ±20%.…”

Determination of ethinyl estradiol and levonorgestrel in human plasma with prednisone as internal standard using ultra-performance liquid chromatography–tandem mass spectrometry

“…Calibration curve was calculated with weighted linear curve fit equation, 1/ x . [9] Calibration curves were considered acceptable when the correlation coefficient ( r ) was greater than 0.98 for biological matrix[10] and the bias of the calculated concentrations was within ±15% of the nominal concentrations, except the LLOQ with an allowed deviation of ±20%. [8]…”