A validated ultra-performance liquid chromatography mass spectrometric method (UPLC–MS/MS) was used for the simultaneous quantitation of candesartan (CN) and hydrochlorothiazide (HCT) in human plasma. The analysis was performed on UPLC–MS/MS system using turbo ion spray interface. Negative ions were measured in multiple reaction monitoring (MRM) mode. The analytes were extracted using a liquid–liquid extraction (LLE) method by using 0.1 mL of plasma volume. The lower limit of quantitation for CN and HCT was 1.00 ng/mL whereas the upper limit of quantitation was 499.15 ng/mL and 601.61 ng/mL for CN and HCT respectively. CN d4 and HCT-13Cd2 were used as the internal standards for CN and HCT respectively. The chromatography was achieved within 2.0 min run time using a C18 Phenomenex, Gemini NX (100 mm×4.6 mm, 5 µm) column with organic mixture:buffer solution (80:20, v/v) at a flow rate of 0.800 mL/min. The method has been successfully applied to establish the bioequivalence of candesartan cilexetil (CNC) and HCT immediate release tablets with reference product in human subjects.
A highly sensitive, selective, and precise ultra-performance liquid chromatography tandem mass spectrometry method was developed and validated for simultaneous quantification of itraconazole and hydroxy itraconazole in human plasma by a single liquid–liquid extraction step. The precursor to product ion transitions of m/z 705.3/392.3, m/z 721.2/408.3 and m/z 708.2/435.4 were used to detect and quantify itraconazole, hydroxy itraconazole and itraconazole-d3 respectively. The lower limit of quantitation was found to be 0.500 ng/mL for itraconazole and 1.00 ng/mL for hydroxy itraconazole. The mean recoveries for itraconazole and hydroxy itraconazole were found to be 100.045% and 100.021%, respectively. This developed method with a chromatographic run time of 2.0 min was successfully applied to a bioequivalence study of 100 mg itraconazole capsule.
Background:The use of anti-histaminic agents has been increased significantly from last decades and till now no method is available for quantitation of ALZ in human plasma which can be applied in a bioequivalence study using LC-MS/MS.Objective:The present study is concerned with the development and validation of ALZ in human plasma by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS).Materials and Methods:Sample preparation involved the extraction with liquid-liquid extraction method by using ethyl acetate as an organic solvent. Chromatographic separation was performed on Atlantis® T3 5 μm 4.6 mm × 150 mm column with the mobile phase consisting of acetonitrile: (10 mm ammonium formate buffer: Formic acid: 99.9:00.1 v/v) 50:50 v/v. The interface used with the application programming interface 4000 LC-MS/MS was a turbo ion spray in which positive ions were measured in multiple reaction monitoring mode. The precursor to product ions transition of m/z 299.30 → 100.20 amu and 305.30 → 106.30 amu were used for ALZ and ALZ D6 respectively.Results:The method was validated over the concentration range of 20.013-10006.551 pg/mL. The mean percent recovery of ALZ was found 77.771% with a precision of 7.71% and the lower limit of quantification was 20.013 pg/mL. The intra- and inter-day precision of the method at three concentrations was 0.98-4.50% and 1.57-5.72% while the intra- and inter-day % accuracy was 99.02-93.82% and 101.78-106.96%. Stability of compounds was established in a series of stability studies. The application of this method was demonstrated in the bioequivalence study and was found suitable in a study of sample size as big as 30 enrolled volunteers.Conclusion:For the very first time, a sensitive, selective and robust Liquid Chromatography- Mass Spectrometry method for the determination of alimemazine (ALZ) in human plasma has been developed and validated using ALZ D6 as an internal standard.
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