A Rapid LC-ESI-MS/MS Method for the Quantitation of Salicylic Acid, an Active Metabolite of Acetylsalicylic Acid: Application to in vivo Pharmacokinetic and Bioequivalence Study in Indian Healthy Male Volunteers

Halder, Dhiman; Dan, Shubhasis; Biswas, Easha; Sarkar, Pradipta; Halder, Umesh Chandra; Pal, Tapan Kumar

doi:10.2174/2213476x03666151105185505

Cited by 9 publications

(3 citation statements)

References 0 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…In this study, we have used hydrochlorothiazide as the IS, because it is a compound structurally similar to ASA; by using hydrochlorothiazide as the IS, a clean peak could be obtained without interference, with a fast detection time with proper retention time similar to those of ASA [ 26 ]. In addition, the analysis of ASA with hydrochlorothiazide as the IS showed that it was possible to detect low concentrations of ASA by optimizing the solvent buffer and column, and the fast detection time had the advantage of accelerating the time required for the analysis.…”

Section: Discussionmentioning

confidence: 99%

Stability of acetylsalicylic acid in human blood collected using volumetric absorptive microsampling (VAMS) under various drying conditions

Moon

Han

Kwak

et al. 2022

Transl Clin Pharmacol

View full text Add to dashboard Cite

Acetylsalicylic acid (ASA) is one of the most commonly used medications in global market, with a risk of intoxication in certain patients. However, monitoring blood drug concentration often requires frequent hospital visits; hence there is an unmet need to increase patient-centricity by conducting blood sampling at home. Volumetric absorptive microsampling (VAMS) is a device that allows collection of homogenous and accurate volume of blood without venipuncture, and can be utilized by patients who are not in hospital settings; but because ASA is prone to hydrolysis and stabilizing reagents cannot be added to VAMS samples, a way to improve sample stability must be developed. The objective of this study was to identify the cause of instability with ASA samples collected by VAMS, and to evaluate ways to improve sample stability. A liquid chromatography with tandem mass spectrometry (LC-MS/MS) was used for analysis of ASA concentration in whole blood. Samples collected with VAMS were kept under different drying conditions (desiccator, pressurized, nitrogen gas and household vacuum sealer) and were compared to the control samples collected by conventional venous sampling. The recovery of ASA was about 31% of the control when VAMS sample was dried at room temperature, whereas VAMS samples under humidity controlled conditions showed more than 85% of recovery. Our results suggest that adequate level of humidity control was critical to ensure sample stability of ASA, and this humidity control could also be achieved at home using household vacuum sealer, thus enabling patient-centric clinical trials to be conducted.

show abstract

Section: Discussionmentioning

confidence: 99%

Stability of acetylsalicylic acid in human blood collected using volumetric absorptive microsampling (VAMS) under various drying conditions

Moon

Han

Kwak

et al. 2022

Transl Clin Pharmacol

View full text Add to dashboard Cite

show abstract

“…The developed and validated LC−ESI−MS/MS assay method was applied to compare the bioavailability of two formulations of EPL by conducting the single oral dose, open label, randomized, two period, two sequence, crossover study [ 27 ] of 30 healthy Indian volunteers (male) with a mean age of 27.53 years (range 21–34 years), mean body weight of 60.23 kg (range 54–66 kg) and mean body height of 168.30 cm (range 162–174 cm) under fasting condition. After an overnight fasting period (10 h), each volunteer was administered either single dose of test preparation of EPL 20 mg Tablet (containing EPL maleate 20 mg, manufactured by JV LLC ‘Pharmland,’ The Republic of Belarus) or reference preparation Renitec 20 mg Tablet (containing EPL maleate 20 mg, manufactured by Merck Sharp & Dohme B.V., The Netherlands) with 240 ml of water, in the sequence determined by randomization.…”

Section: Methodsmentioning

confidence: 99%

LC–MS/MS Assay for Quantitation of Enalapril and Enalaprilat in Plasma for Bioequivalence Study in Indian Subjects

Halder

Dan

Pal³

et al. 2017

Future Sci. OA

Self Cite

View full text Add to dashboard Cite

Background:Enalapril (EPL) is an angiotensin-converting enzyme inhibitor for the treatment of hypertension and chronic heart failure. Enalaprilat (EPLT) is an active metabolite that contributes to the overall activity of EPL.Aim:To quantitate EPL along with its metabolite EPLT using LC–MS/MS, a bioanalytical method was developed and validated with tolbutamide in human plasma using a protein precipitation technique.Results:The sensitive and selective method has an LLOQ of 1 ng/ml with a linearity range of 1–500 ng/ml for both EPL and EPLT using 300 µl of plasma without any matrix effect.Conclusion:Linearity, specificity, accuracy, precision and stability, as well as its application to the analysis of plasma samples after oral administration of 20 mg of EPL maleate in healthy volunteers demonstrate applicability to bioavailability/bioequivalence studies.

show abstract

“…For this open label, randomized, two period, two sequence, crossover study, [24][25][26][27] 24 healthy Indian volunteers (male) with a mean age of 25.23 AE 5.41 years and a mean body weight of 65.60 AE 3.64 kg have been selected. After an overnight fasting period (10 h), each volunteer was given either single dose of test preparation tablet (containing NSD 100 mg, manufactured by Pharmland JV Leninskaja STR, 124, 222603, Nesviz Belarus) or reference preparation tablet Nise (containing NSD 100 mg, manufactured by Dr. Reddy's Laboratories Ltd, Solan, India) with 240 mL of water, in the sequence determined by randomization.…”

Section: Bioequivalence Study and Pharmacokinetic Parametersmentioning

confidence: 99%

LC-MS/MS determination of 4-hydroxynimesulide, an active metabolite of nimesulide and application to bioequivalence study in Indian subjects

Halder

Dan

Sarkar

et al. 2019

Eur J Mass Spectrom (Chichester)

Self Cite

View full text Add to dashboard Cite

A simple and highly sensitive bioanalytical method was developed and validated for simultaneous quantification of nimesulide (NSD) and its active metabolite 4-hydroxy-nimesulide (M1) in human plasma by liquid chromatography-tandem mass spectrometer (LC-MS/MS) and applied in a bioequivalence study performed on Indian subjects. The bioanalytical method was carried out by LC-MS/MS with celecoxib (CXB) as an internal standard (IS) using liquid–liquid extraction technique. The chromatographic separation was performed on a reversed-phase Agilent eclipse plus C18 (75 mm × 4.6 mm, particle size 3.5 µm) column with a mobile phase of acetronitrile and water containing 5 mM ammonium formate (9:1, v/v). Method validation and clinical sample were analysed as per USFDA and EMA guidelines and results met the acceptance criteria. The lower limit of quantitation of NSD and M1 was found 10 ng/mL with a large linearity range from 10 to 6000 ng/mL for both NSD and M1 using only 100 µL of plasma and reported no matrix effect. The multiple reaction monitoring transitions of m/z 307.20 → 229.20, m/z 323.00 → 245.00 and m/z 380.20 → 316.20 were used to measure NSD, M1 and CXB (IS), respectively. The assay method was successfully applied for the simultaneous quantification of both NSD and M1 in plasma samples after oral administration of nimesulide 100 mg tablet in healthy human subjects.

show abstract

A Rapid LC-ESI-MS/MS Method for the Quantitation of Salicylic Acid, an Active Metabolite of Acetylsalicylic Acid: Application to in vivo Pharmacokinetic and Bioequivalence Study in Indian Healthy Male Volunteers

Cited by 9 publications

References 0 publications

Stability of acetylsalicylic acid in human blood collected using volumetric absorptive microsampling (VAMS) under various drying conditions

Stability of acetylsalicylic acid in human blood collected using volumetric absorptive microsampling (VAMS) under various drying conditions

LC–MS/MS Assay for Quantitation of Enalapril and Enalaprilat in Plasma for Bioequivalence Study in Indian Subjects

LC-MS/MS determination of 4-hydroxynimesulide, an active metabolite of nimesulide and application to bioequivalence study in Indian subjects

Contact Info

Product

Resources

About