Development and validation of a bio-analytical method for simultaneous quantification of nebivolol and labetalol in aqueous humor and plasma using LC-MS/MS and its application to ocular pharmacokinetic studies

2020 ◽  
Vol 1136 ◽  
pp. 121908
Author(s):  
Pradeep Singh Rawat ◽  
Punna Rao Ravi ◽  
Laxman Kaswan ◽  
Rajeev Singh Raghuvanshi
2021 ◽  
Vol 89 (1) ◽  
pp. 8
Author(s):  
Jorge Cruz-Angeles ◽  
Luz María Martínez ◽  
Marcelo Videa ◽  
José Rodríguez-Rodríguez ◽  
Cecilia Martínez-Jiménez

Worldwide, 25% of the population suffers from metabolic syndrome (MetS). The treatment of patients with MetS regularly includes drugs prescribed simultaneously to treat several disorders that manifest at the same time, such as hypercholesterolemia, arterial hypertension, and diabetes. To the authors’ best knowledge, there is no previous published analytical method for the simultaneous quantification of drugs used in the treatment of these diseases. In the present study, a rapid high-performance liquid chromatography with a diode-array detector HPLC-DAD methodology was developed for simultaneous quantification of carvedilol (CVD), telmisartan (TEL), bezafibrate (BZT), gliclazide (GZD), and glimepiride (GMP) in bulk and pharmaceutical form. The chromatographic separation of the five pharmaceuticals was achieved on a Hypersil GOLD C18 Selectivity (5 µm, 150 × 4.60 mm2) using a mobile phase of acetonitrile (50%) and 0.02 M KH2PO4, pH 3 (50%) at a flow rate of 1 mL/min and at 25 °C. The total separation time was 9 min. The analytical method was validated following the International Conference on Harmonization guidelines. A reproducible method was obtained with acceptable limits of detection (LOD) and quantification (LOQ) for CVD (0.012 and 0.035 μg mL−1), TEL (0.103 and 0.313 μg mL−1), BZT (0.025 and 0.076 μg mL−1), GZD (0.039 and 0.117 μg mL−1), and GMP (0.064 and 0.127 μg mL−1). The validated method allowed the determination of these drugs in commercial pharmaceutical products both individually and simultaneously. The present method was found to be suitable for simultaneous quantification of the five drugs that are most commonly used in the simultaneous treatment of the metabolic syndrome.


Medicines ◽  
2019 ◽  
Vol 6 (1) ◽  
pp. 36 ◽  
Author(s):  
Vito Taddeo ◽  
Ulises Castillo ◽  
Morena Martínez ◽  
Jenny Menjivar ◽  
Ignacio Jiménez ◽  
...  

Background: Quinonemethide triterpenoids, known as celastroloids, constitute a relatively small group of biologically active compounds restricted to the Celastraceae family and, therefore, they are chemotaxonomic markers for this family. Among this particular type of metabolite, pristimerin and tingenone are considered traditional medicines in Latin America. The aim of this study was the isolation of the most abundant celastroloids from the root bark of Maytenus chiapensis, and thereafter, to develop an analytical method to identify pristimerin and tingenone in the Celastraceae species. Methods: Pristimerin and tingenone were isolated from the n-hexane-Et2O extract of the root bark of M. chiapensis through chromatographic techniques, and were used as internal standards. Application of a validated RP HPLC-PDA method was developed for the simultaneous quantification of these two metabolites in three different extracts, n-hexane-Et2O, methanol, and water, to determine the best extractor solvent. Results: Concentration values showed great variation between the solvents used for extraction, with the n-hexane–Et2O extract being the richest in pristimerin and tingenone. Conclusions: M. chiapensis is a source of two biologically active quinonemethide triterpenoids. An analytical method was developed for the qualification and quantification of these two celastroloids in the root bark extracts of M. chiapensis. The validated method reported herein could be extended and be useful in analyzing Celastraceae species and real commercial samples.


2020 ◽  
Vol 16 (8) ◽  
pp. 979-987
Author(s):  
Edgar Alejandro de Leon-Diaz de Leon ◽  
Antonio Gordillo-Moscoso ◽  
Úrsula Medina ◽  
Ángel Antonio Vertiz Hernández ◽  
Rafael Almendra-Pegueros ◽  
...  

Background: Losartan, one of the most frequently used drugs in Heart Failure (HF) treatment, could be modified for its bioavailability (BA) by generic formulations and other factors. Hence, the importance of therapeutic drug monitoring. Objective: Development and validation of a simplified analytical method using HPLC for simultaneous quantification of losartan and E-3174 in human plasma samples. The method was tested for determining the pharmacokinetics parameters of HF patients. Methods: Analytical conditions were optimized using a C18 column (4.6 X 50 mm, 3 μm. Thermo Scientific) at 25ºC. Conditions of mobile phase: a phosphate buffer (0.01M), adjusted to pH 2.5 with phosphoric acid (1M) and Acetonitrile (60:40 v/v). The flow rate was maintained at 1.2 mL/min, on a running time of 5 min and a sample injection volume of 50 μL. Absorbance for measurement of losartan and E-3174 was 200 nm. Pharmacokinetics profiles were determined with Phoenix Win- Nonlin 8.1 software in a non-compartmental model. Results: Analytical method developed and validated in this work is precise and accurate for simultaneous determination of losartan and E-3174 in human plasma samples in a range of 0.02 -10 μg/mL. In HF subjects, lower Tmax and higher Cmax for losartan and E-3174 patent than generic formulation were observed, which can be translated into less biological effect and more time to present it by the generic drug. Conclusion: The pharmacokinetic profile is dependent on the type of formulation studied (generic/ patent) hence the importance of conducting evaluations in our patients to ensure that the expected therapeutic effect is achieved with treatment administered.


2019 ◽  
Vol 8 (3) ◽  
pp. 79-84
Author(s):  
E. N. Fisher ◽  
E. S. Melnikov ◽  
I Е. Shohin

Introduction. Busereline, being a synthetic gonadotropin-releasing hormone analog, is widely used for hormone-dependent cancer treatment (e.g. prostate cancer and breast cancer). Based on the accumulated scientific data for busereline quantitation in biosamples, the main analytical method that is used for this purpose is high-performance liquid chromatography (HPLC) with fluorescence detection, combined with protein precipitation (TCA 10%) for sample preparation. However, due to several limitations of this method resulting in low sensitivity (at the µg/mL level of concentrations), the HPLC-MS/MS analytical method was chosen for peptide determination in biosamples. The HPLC-MS/MS method is considered to have higher accuracy and specificity. The main sample preparation method for gonadotropin-releasing hormone analogs is solid-phase extraction. In our work, we’ve chosen protein precipitation as an alternative – easier and less laborious biosamples preparation process.Aim. The main objective of this study was the development and validation of HPLC-MS/MS method for busereline quantitation in animal (mini pigs) plasma samples and its further application to pharmacokinetic studies.Materials and methods. Busereline quantitative determination in plasma samples was performed using HPLC-MS/MS method. A protein precipitation procedure (methanol, 1:2, v/v) was used for busereline extraction from pig plasma.Results and discussion. The developed analytical method was validated for selectivity, linearity, matrix effect, accuracy (intra-day, inter-day), precision (intra-day, inter-day), LLOQ, carryover and stability.Conclusion. A new HPLC-MS/MS method for busereline quantitation in blood plasma was developed and successfully validated. The developed method showed linearity over the quantitation range from 1 to 20 ng/mL. The developed method can be successfully applied to busereline pharmacokinetic studies.


2017 ◽  
Vol 9 (22) ◽  
pp. 3329-3337 ◽  
Author(s):  
Jr-Ting Lee ◽  
Li-Heng Pao ◽  
Chang-Da Hsieh ◽  
Pei-Wei Huang ◽  
Oliver Yoa-Pu Hu

A simple and sensitive method for the determination of hesperidin and hesperetin was necessary for a pharmacokinetic (PK) study in Wistar rats.


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