Objective
The aim of the work was to develop and validate a simple, sensitive and selective Liquid chromatography with Mass spectroscopic method for simultaneous quantification of lidocaine and prilocaine in human plasma.
Design and methods
Analytes and the internal standards from human plasma were extracted by using solid- phase extraction technique using Waters Oasis® HLB 1 cc (30 mg) cartridges. The reconstituted samples were chromatographed on Phenomenex Kinetex EVO 4.6*100 mm 2.6 μ 100A column by using a mixture of acetonitrile and 5 mM ammonium acetate buffer (80:20, v/v) as the mobile phase at a flow rate of 0.6 mL/min.
Results
The method was validated over the concentration range of 0.10–201.80 ng/mL for lidocaine and 0.10–201.66 ng/mL for prilocaine. The calibration curve obtained was linear.
Conclusion
Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 3.0 min for each sample, make it possible to analyze more than 350 human plasma samples per day. The proposed method was found applicable for pharmacokinetic studies.
There has been much research on both saxagliptin and dapagliflozin. However, only a few HPLC and LC-MS methods that use stable labeled isotopes to measure the amount of a drug alone or in combination with other drugs and have a longer chromatographic run time have been published. A quick and sensitive LC-MS/MS mass spectrometric test method has been made and fully validated to find dapagliflozin and saxagliptin in human plasma simultaneously. Solid-phase extraction on the Cleanert PEP-H extraction cartridge was used to separate the analyte and I.S. from the human plasma. The extracted samples were separated on an Ace Phenyl (150 X 4.6 mm, 5 m) column at a set flow rate of 0.8 mL/min using an isocratic mobile phase of acetonitrile and 5 mM ammonium acetate buffer (70:30 v/v). For dapagliflozin, the calibration curve was linear throughout a range of 0.502-227 ng/mL, while for saxagliptin, the range was 0.103-76.402 ng/mL. The procedure was validated in accordance with standards set by the U.S. Food and Drug Administration, and the outcomes are acceptable.
A highly sensitive, specific and rapid liquid chromatography-tandem mass spectrometry technique for the quantification of tasimelteon in human plasma has been developed and validated using tasimelteon-d 5 as internal standard. Liquid-liquid extraction technique with ethyl acetate was used for extraction of tasimelteon from the plasma.The chromatographic separation was achieved on an Agilent Zorbax, Eclipse, C 18 (4.6 × 50 mm, 5 μm) column using a mobile phase of acetonitrile and 0.02% formic acid buffer (85:15, v/v) with a flow rate of 0.5 mL/min. A detailed method validation was performed as per the United States Food and Drug Administration guidelines. The linear calibration curve was obtained over the concentration range 0.30-299 ng/mL. The API-4000 liquid chromatography-tandem mass spectrometry was operated under multiple reaction monitoring mode during analysis. The validated method was successfully applied to estimate plasma concentration of tasimelteon after oral administration of a single dose of a 20 mg capsule in healthy volunteers under fasting conditions. The maximum concentration of the drug achieved in the plasma was 314 ± 147 ng/mL and the time at which this concentration was attained was 0.54 ± 0.22 h.
The aim of this work was to develop a simple,sensitive and selective liquid chromatography tandem mass spectrometry assay for quantification ofmoexipril in human plasma. Analytes and the internal standard(stable labelled isotopes) from human plasma by using solid-phase extraction technique with the help of Waters Oasis ® HLB 1 cc (30 mg) extraction cartridge. The reconstituted samples were chromatographed on Zorbax XDB C18,4.6*50mm column by using a mixture of acetonitrile -5 mM ammonium acetate buffer (80:20, v/v)as the mobile phase at a flow rate of 0.6 mL/min.The calibration curve obtained was linear (r 0.99) over the concentration range of 0.102-101.389 ng/mL for moexipril. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.2 min for each sample made it possible to analyze more than 350 human plasma samples per day.
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