scholarly journals Development and Validation of a Rapid Analytical Method for the Simultaneous Quantification of Metabolic Syndrome Drugs by HPLC-DAD Chromatography

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.

Author(s):  
SENTHIL RAJAN D. ◽  
MURUGANATHAN G. ◽  
KUMUTAAVALLI SHIVKUMAR ◽  
GANESH THANGAVEL

Objective: The present study was undertaken to develop a rapid, simple, specific and economic high performance liquid chromatographic (HPLC) method has been developed, validated and used for simultaneous quantification of Vasicine, Glycyrrhizin and Piperine in poly herbal cough syrup Methods: An Agilent technologies 1200 Series quaternary pump combined with an Agilent 1200 series photo diode array detector (USA), an Agilent 1200 series vacuum degasser (USA) and an Agilent autosampler injector. Chromatographic separation was performed on a Hiber, prepacked column, C18, Size 250x 4.60 mm, 5µ maintained at 25 °C. PJ (solvent A) and HPLC grade Acetonitrile (solvent B). Results: The HPLC developed for quantization was simple, accurate and specific. The drug follows the beer’s lambert’s law in the concentration range of of Vasicine in concentration range 25–250 μg/ml, glycyrrhizin in concentration range 100–1000 μg/ml and Piperine in concentration range of 20–100μg/ml and exhibited good correlation coefficient and excellent mean recovery. Percentage RSD for precision and accuracy of the method was found to be less than 2%. Conclusion: The present standardization provides a specific and rapid tool in the herbal research, permitting to set quality specifications for identity, transparency and reproducibility of these Phytoconsituents in the herbal Cough syrup.


2013 ◽  
Vol 96 (3) ◽  
pp. 670-675 ◽  
Author(s):  
Balwinder Singh ◽  
Kousik Mandal ◽  
Sanjay K Sahoo ◽  
Urvashi Bhardwaj ◽  
Raminderjit Singh Battu

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.


2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.


2019 ◽  
Vol 19 (1) ◽  
Author(s):  
Olimpia Arellano-Campos ◽  
Donaji V. Gómez-Velasco ◽  
Omar Yaxmehen Bello-Chavolla ◽  
Ivette Cruz-Bautista ◽  
Marco A. Melgarejo-Hernandez ◽  
...  

Author(s):  
BAITHA PALANGGATAN MAGGADANI ◽  
JIHAN YASMINA ◽  
HARMITA HARMITA

Objective: Whitening cream is a cosmetic that contains ingredients that can alleviate hyperpigmentation. Tranexamic acid (TA) is one of the potentialanti-pigmentation agents that work through inhibiting plasmin. TA is used in cosmetic formulations at a concentration of 2.5% as a whitening andmoisturizing agent. To date, research on TA in both cosmetics and other pharmaceutical products using high-performance liquid chromatography(HPLC) has not been done directly (without derivatization). Therefore, this study aimed to develop a simple and rapid analytical method for TA(without derivatization) in cosmetic cream samples using reverse-phase HPLC and water as a solvent.Methods: Optimization was conducted by evaluating several parameters that affect sample extraction, as well as composition and mobile phasetypes. The optimal method must fulfill suitability and validation requirements. The optimal method should be able to detect and quantify TA in creamsamples without derivatization.Results: The optimal analysis condition used a ultraviolet detector at a wavelength of 210 nm, acetonitrile: double-distilled water: phosphoric acid(64:34:2) as the mobile phase and a flow rate of 0.8 mL/min. The retention time of the analyte occurred in the 2nd min.Conclusion: The analytical method that met the validation requirements was characterized using parameters such as accuracy, precision, linearity,selectivity, limit, of detection, and limit of quantitation. This method is applicable for analyzing TA content in samples with a concentration of 1.02%.


Author(s):  
Agna Heliade Oliveira ◽  
Valmir Gomesde Souza ◽  
FÁbio Santosde Souza ◽  
Rui Oliveira Macedo

Objective: This study aims to develop the extraction of the marker kaempferol in the fluid extract (FE) and validate an analytical method that monitors the quality of extracts of P. pyramidalis. Methods: The P. pyramidalis leaves were collected and then were dried to milling process. The extracts were drawn up at 20% weight: Volume (w/v) by maceration, and the extraction system used was hydroethanol solution ratio at 50:50 volume: Volume (v: v). From the hydroalcoholic extract, a method of extracting the kaempferol biomarker was developed and validated by high-performance liquid chromatography coupled with diode array detector. To validate a method, the following parameters were evaluated: Specificity, selectivity, linearity, limit of quantification (LOQ) and detection (LOD), precision, accuracy, robustness, and stability. Results: The method developed proved to be efficient, as it allowed the analysis of the interferents free marker, with recovery above 90%, linear over the range 1.4–26.6 μg/mL, correlation coefficient R2=0.999, and LOD and LOQ 0.07 and 0.22 μg/mL, respectively, specificity, precision, accuracy, and robustness. Conclusion: The extraction methodology of the kaempferol marker was successfully developed interferents free and the validated method by HPLC-DAD represents a useful tool in the quality control of P. pyramidalis herbal medicines.


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