scholarly journals Stability indicating RP-UPLC method development and validation for the simultaneous determination of ertugliflozin and metformin in plasma

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 2417-2424
Author(s):  
Haritha G ◽  
Shanmugasundaram P
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Internal Standard ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Method Development And Validation ◽  
Resultant Solution ◽  
The Stability ◽  
Development And Validation

New stability-indicating RP-UPLC technique was developed for the quantification of ertugliflozin and metformin  in human plasma and validated as per the regulatory guidelines. Both the drug components and internal standard were spiked to blank plasma and subjected to liquid-liquid extraction with the mobile phase. The resultant solution was infused into Acquity BEH-C18 (1.7 μ, 100×2.1mm) non-polar column comprising NaH2PO4  buffer (pH-3.5), methanol and acetonitrile in the ratio of 50:10:40% v/v/v  as mobile phase. The detector response and flow of the mobile phase were monitored at 240nm and 0.5ml/min, respectively. The linearity plot was made in the concentration range of 0.1-3.0 µg/ml for metformin and 0.05-1.5 µg/ml for ertugliflozin with correlation coefficient value of more than 0.999. The developed method was subjected for bench-top, freeze and thaw, long-term and short-term stability studies and the drug components were stable over the respective conditions. The Lower limit of quantification (LLOQ) for ertugliflozin and metformin  were 0.05 and 0.1 µg/ml, respectively. The findings of precision and accuracy were present in between 2.6 to 4.2 %RSD and -2 to 3.99 %RE, respectively. The findings of the stability data were presented below. The %stability of ertugliflozin and metformin  were varying from 96% to 104% for ertugliflozin and 96% to 105% for metformin.

scholarly journals BIO-ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF AVELUMAB, AXITINIB AND ITS APPLICATION TO PHARMACOKINETIC STUDIES IN RABBIT PLASMA BY USING LCMS/MS

2021 ◽  
pp. 198-204
Author(s):  
SYED RAFI ◽  
KANTIPUDI RAMBABU
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Internal Standard ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Stability Results ◽  
Good Agreement

Objective: An easy, quick, precise, active and reproducible LC-MS/MS technique was developed for the bioanalytical method of Avelumab and Axitinib using Cytarabine as an internal standard. Methods: This article summarizes the recent progress on bioanalytical LC-MS/MS methods using waters x-bridge phenyl column (150x4.6 mm, 3.5µ) column and organic mobile phase of 0.1% Tri fluoro acetic acid and Acetonitrile in 50:50 ratio. Results: The calibration curve was linear in the range of 2-40 ng/ml for avelumab and 0.5-10 ng/ml axitnib. Accuracy, precision, recovery, matrix effect and stability results were found to be within the suitable limits. Simple and efficient method was developed and utilized in pharmacokinetic studies to see the investigated analyte in body fluids. Conclusion: The application denotes all the parameters of system suitability, specificity, linearity and accuracy are in good agreement with USFDA guidelines and applied effectively for the investigation of pharmacokinetic studies in rabbit.

scholarly journals Method Development And Validation For Estimation Of Commercially Produced Sex Pheromones In Lure

2013 ◽  
Vol 25 (2) ◽  
pp. 180-185
Author(s):  
Shankar Mandal ◽  
AMH Rahman ◽  
MIR Mamun ◽  
Mohammad Shoeb ◽  
Nilufar Nahar
Keyword(s):  
Sex Pheromones ◽  
Method Development ◽  
Limit Of Detection ◽  
Chemical Society ◽  
Methyl Eugenol ◽  
Technical Grade ◽  
Limit Of Quantification ◽  
Method Development And Validation ◽  
The Stability ◽  
Development And Validation

A method was developed and validated for quantitation of methyl eugenol and cuelure, the active ingredients of two formulated sex pheromones (bio-pesticides) Mukti and Jhilik by gas chromatography. Technical grade methyl eugenol and cuelure (purity 95- 96%) were used as standards. Calibration curves of methyl eugenol and cuelure were linear with correlation coefficient (r2) 0.9966 & 0.9988, respectively. Ten replicate analyses were done for both methyl eugenol & cuelure and quantity of the pheromones in the two formulated products were found to be 0.55 ± 0.11 and 0.56 ± 0.09 g/lure (Mean ± SD), respectively. The stability of both pheromones in solution and their diffusion from lures under UV-Vis light was determined for a period of 21 days. The results showed that diffusion of the both pheromones from lure were very fast and about two-third diffused within 10 days after exposure. Methyl eugenol was quite stable in solution, whereas cuelure was found to degrade slowly, and about 15 % cuelure degraded within 21 days. The recovery of methyl eugenol and cuelure from matrix were found to be 80.69 ± 3.14 and 78.48 ± 4.32 % (mean ± SD), respectively, where limit of detection (LOD) & limit of quantification (LOQ) were found to be 97 & 80 ppm, and 290 & 240 ppm, respectively. The developed method is very simple and can be used for estimation of the two sex pheromones. Journal of Bangladesh Chemical Society, Vol. 25(2), 180-185, 2012 DOI: http://dx.doi.org/10.3329/jbcs.v25i2.15084

High Performance HPLC-UV Method Development and Validation for Sulfadoxine from its Potential Interfering Impurities

2021 ◽  
Vol 08 ◽  
Author(s):  
Nayan S. Gadhari ◽  
Jayram V. Gholave ◽  
Suyog S. Patil ◽  
Ajay R. Patil ◽  
Kiran F. Shelke ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Degradation Products ◽  
Drug Product ◽  
Ich Guidelines ◽  
Daunting Task ◽  
Method Development And Validation ◽  
The Stability ◽  
Development And Validation

Objective: To address the separation of interfering potential impurities associated with the drug is always a daunting task. We present the method validation and quantitative determination of sulfadoxine (SUL), an anti-malarial drug with most important interfering impurities present pharmaceutical dosages and in bulk samples using HPLC-UV method. Methods: The UV detection was obtained at 270 nm and SUL is separated on Sunfire C18 (25 cm x 4.6 mm x 5 µ m) column at 45°C with flow rate of 1.0 mL/min in a mobile phase (CH3COOH:CH3CN). The stress testing (acidic/basic/oxidative) was performed using HPLC for SUL and its impurities showing the highly efficient separation peaks between degradant and drug product. Results: The developed method was found to be highly accurate and sensitive in regulation with ICH guidelines. Also, it was found to be free from interference from degradation products which allows the stability indicating capability of developed HPLC-UV method for SUL for validation in bulk drugs. Conclusion: The main advantages of the present method; (a) Separation achieved in 30 minutes, (b) MS compatible mobile phase renders this developed method can be directly adapted to LC-MS without any major modifications in near future, and (c) separation of twelve impurities on Sunfire C18 column. The CFs (correction factors) had been calculated for all the impurities. It was found to be 1.6 (IMP IX), 1.70 (IMP XI) and in between 0.8-1.3 for all other impurities. The LOD of the developed method for all the analytes were in the range of 0.05 to 0.11 μg/mL and the LOQ values were in the range of 0.17 to 0.36 μg/mL.

scholarly journals Bioanalytical method development and validation for determination of metoprolol tartarate and hydrochlorothiazide using HPTLC in human plasma

2013 ◽  
Vol 49 (4) ◽  
pp. 845-851 ◽  
Author(s):  
Ambadas Ranganath Rote ◽  
Poonam Ramdas Sonavane
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Internal Standard ◽  
Analytical Technique ◽  
Method Development And Validation ◽  
Rf Values ◽  
The Stability ◽  
Development And Validation

A simple, sensitive, rapid and economic chromatographic method has been developed for determination of metoprolol tartarate and hydrochlorothiazide in human plasma using paracetamol as an internal standard. The analytical technique used for method development was high-performance thin-layer chromatography. HPTLC Camag with precoated silica gel Plate 60F254 (20 cm×10 cm) at 250 µm thicknesses (E. Merck, Darmstadt, Germany) was used as the stationary phase. The mobile phase used consisted of chloroform: methanol: ammonia (9:1:0.5v/v/v). Densitometric analysis was carried out at a wavelength of 239 nm. The rf values for hydrochlorothiazide, paracetamol and metoprolol tartarate were 0.13±0.04, 0.28±0.05, 0.48±0.04, respectively. Plasma samples were extracted by protein precipitation with methanol. Concentration ranges of 200, 400, 600, 800, 1000, 1200 ng/mL and 2000, 4000, 6000, 8000, 10000, 12000 ng/mL of hydrochlorothiazide and metoprolol tartarate, respectively, were used with plasma for the calibration curves. The percent recovery of metoprolol tartarate and hydrochlorothiazide was found to be 77.30 and 77.02 %, respectively. The stability of metoprolol tartarate and hydrochlorothiazide in plasma were confirmed during three freeze-thaw cycles (-20 ºC) on a bench for 24 hours and post-preparatively for 48 hours. The proposed method was validated statistically and proved suitable for determination of metoprolol tartarate and hydrochlorothiazide in human plasma.

Bioanalytical Method Development and Validation for the Determination of Vasopressin Receptor Antagonist Conivaptan in Mouse Plasma at NanoLevel and its Pharmacokinetic Application

2019 ◽  
Vol 15 (5) ◽  
pp. 591-598 ◽  
Author(s):  
Haitham Alrabiah ◽  
Ahmed Bakheit ◽  
Sabray Attia ◽  
Gamal A.E. Mostafa
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Vasopressin Receptor ◽  
Mouse Plasma ◽  
Precipitation Procedure ◽  
Validation Parameters ◽  
The Us ◽  
Method Development And Validation ◽  
Development And Validation

Background: Conivaptan inhibits two of vasopressin receptor (vasopressin receptor V1a and V2). Conivaptan is used for the treatment of hyponatremia, and in some instances, for the treatment of the heart failure. Methods: The present study aimed to develop a simple, sensitive, and accurate HPLC with ultraviolet detection for the assay of conivaptan (CON) in mouse plasma using bisoprolol as internal standard (IS). A precipitation procedure was used to extract CON and the IS from the mouse plasma. CON was chromatographically separated using a C18 analytical column at 25°C. The separation was carried out using a mixture of phosphate buffer (50 mM): acetonitrile (60: 40, v/v, pH 4.5) with a flow rate of 1.0 mL/min and detection was performed at 240 nm. Results: The assay was validated according to the US Food and Drug (FDA) guidelines. The method demonstrated linearity over a concentration range of 150 - 2000 ng/mL (correlation coefficient: r 2 = 0.9985). The mean recovery of CON from the mouse plasma was 101.13%. All validation parameters for CON were within the acceptable range. Conclusion: The investigated method has been shown to be suitable for estimating the CON in plasma samples, and this method is sensitive and highly selective, allowing the estimation of its concentrations up to the nano-scale. The suggested method was successfully used in a pharmacokinetic study of CON in mouse plasma.

scholarly journals RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

2013 ◽  
Vol 49 (2) ◽  
pp. 359-366 ◽  
Author(s):  
Mustafa Çelebier ◽  
Tuba Reçber ◽  
Engin Koçak ◽  
Sacide Altinöz
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

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