scholarly journals A VALIDATED STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR DACLATASVIR, IDENTIFICATION AND CHARACTERIZATION OF DEGRADATION PRODUCTS USING LC-ESI-QTOF-MS

2019 ◽  
pp. 302-308
Author(s):  
SNEHAL V WARGHADE ◽  
KAILAS G BOTHARA
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Antiviral Drug ◽  
Array Detector ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
The Stability

Objective: The objective of this study was to report the stability of antiviral drug, daclatasvir (DCV) based on the information obtained from forced degradation studies and characterization of degradation products (DPs) by tandem mass spectrometry (MS/MS) analysis. Methods: Chromatographic separation was achieved on Shimadzu liquid chromatography (LC) 20 AD high-performance LC system with photodiode array detector having Kromasil C18 (250 mm×4.6 mm×5 μm) with isocratic elution of a mobile phase composed of ammonium acetate buffer (pH 4.5) and acetonitrile in a ratio of 50:50 at 315 nm. The drug was subjected to forced hydrolytic, oxidative, photolytic, and thermal stress in accordance with the ICH guideline Q1A (R2). The drug showed degradation under acidic and basic hydrolytic conditions by forming two DPs. The DPs were characterized using LC– MS/MS studies and the pathways of fragmentation are proposed. Validation of the developed method was carried out in accordance with ICH guidelines. Results: Two DPs were identified, DP-1 as (S)-1-((S)-2-(5-(4’-(2-((S)-1-((S)-2-((methoxycarbonyl)amino)-3-methylbutanoyl)pyrrolidin-2-yl)-1H-imidazol-5-yl)-[1,1’-biphenyl]-4-yl)-1H-imidazol-2-yl)pyrrolidin-1-yl)-3-methyl-1-oxobutan-2-aminium and DP-2 as (S)-2-(5-(4’-(2-((S)-1-((S)-2- ((methoxycarbonyl)amino)-3-methylbutanoyl)pyrrolidin-2-yl)-1H-imidazol-5-yl)-[1,1’-biphenyl]-4-yl)-1H-imidazol-2-yl)pyrrolidin-1-ium. Conclusion: The method proved to be simple, accurate, precise, specific, robust, and less time consuming and can be applied for the determination of DCV in bulk and marketed formulation.

scholarly journals Development and Validation of a Stability indicating Related Substances of Baricitinib by RP-HPLC and its Degradation

2019 ◽  
Vol 4 (2) ◽  
pp. 4-9
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Array Detector ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Related Substances ◽  
Photodiode Array Detector ◽  
Liquid Chromatography Method ◽  
Hydrolysis Conditions ◽  
Development And Validation

Reverse phase high performance liquid chromatography method, for estimation of related substances or chromatographic impurities of Barcitinib was developed and validated. Baricitinib was developed by separating its degradation products on a X-Terra RP18 (150x4.6mm, 5.0 µm) column using 0.1% Tri ethyl amine in water adjusted pH-2.5 with OPA and Acetonitrile in simple gradient at a flow rate 1.0 ml/min. The column effluents were monitored by a photodiode array detector set at 224nm. The method was validated in terms of specificity, linearity, accuracy, precision, detection limit, quantification limit and robustness. Forced degradation of Baricitinib was carried out under acidic, basic, peroxide, reduction, thermal, photo and hydrolysis conditions. The proposed method is validated as per ICH Q2 (R1) guidelines. The proposed method is simple as selected chromatographic conditions are not so difficult to apply in routine analysis for testing the chromatographic impurity of baricitinib.

scholarly journals STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF APIGENIN AND LUTEOLIN FROM ACHILLEA MILLEFOLIUM LINN

2019 ◽  
pp. 169-172
Author(s):  
GOMATHY SUBRAMANIAN ◽  
S.N.MEYYANATHAN ◽  
GOWRAMMA BYRAN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Objective: A stability-indicating reverse-phase high-performance liquid chromatographic method was developed and validated for the analysis of apigenin and luteolin. The degradation behavior of apigenin and luteolin was investigated under different stress conditions as recommended by the International Conference on Harmonization (ICH). Methods: In the present study, a reversed-phase high-performance liquid chromatography method was developed and the resolution of the plant constituents was successfully achieved using Hibar Lichrospher C8 column with ultraviolet detector at a wavelength of 269 nm. The mobile phase consisted of methanol and 0.5% trifluoroacetic acid (80:20 v/v) at a flow rate of 1.0 ml/min. Both apigenin and luteolin were subjected to various stress degradation studies such as oxidation, acid and alkaline hydrolysis, and photolytic degradation. Results: The proposed method was found to be linear (1–5 μg/ml) with the linear correlation coefficient of R2=0.99. Although the degradation products of stressed conditions were not identified, the methods were able to detect the changes due to stress condition. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. Forced degradation studies on apigenin and luteolin give information about their storage and intrinsic stability conditions considering the advanced pharmaceutical aspects of formulations.

FORCED DEGRADATION STUDY OF ELETRIPTAN BY USING ULTRA HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (UHPLC)

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (07) ◽  
pp. 14-21
Author(s):  
S. Sahu ◽  
◽  
R.M Singh ◽  
S.C. Mathur ◽  
D. K Sharma ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Degradation Study ◽  
Liquid Chromatography Method ◽  
Isocratic Mode

A simple, fast, precise and accurate ultra high performance liquid chromatography method was developed for degradation study of eletriptan hydrobromide (EH) under exaggerated conditions. An Inertsil ODS C18 (250 x 4.6 mm, 5µm) column in isocratic mode was used with mobile phase comprising of water, methanol and trifluoroacetic acid mixed in the ratio 55:45:0.1 % V/V/V, maintained at pH 3.5. The flow rate was set at 0.4 mL per minute with UV detection at 225 nm. The retention time of EH was found to be 3.7 minutes. Linearity for EH was found in the range of 3.5- 200 µg per mL and percentage recoveries were obtained in the range of 100.2 % to 100.6 %. The method was capable of resolving all degradants and principle component in sample. The proposed method is accurate, precise, selective, reproducible, and rapid for detection of degradation of eletriptan hydrobromide.

scholarly journals DEVELOPMENT AND VALIDATION OF AN HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF 17-Β ESTRADIOL IN POLYMERIC NANOPARTICLES

2021 ◽  
pp. 112-116
Author(s):  
ADRIANA YURIKO KOGA ◽  
BRUNA CARLETTO ◽  
LEANDRO CAVALCANTE LIPINSKI ◽  
TRAUDI KLEIN ◽  
PAULO VITOR FARAGO
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Polymeric Nanoparticles ◽  
Chromatography Method ◽  
Limits Of Detection ◽  
Ph Variation ◽  
Liquid Chromatography Method ◽  
The Stability ◽  
Development And Validation ◽  
Detection And Quantification

Objective: A simple high-performace liquid chromatography method was developed and validated to determine 17-β estradiol in poly (ε-caprolactone) nanocapsules. Methods: The chromatographic conditions were as follows: C18 GL column with a mobile phase of acetonitrile:water (92:8 v/v) at flow rate of 1.5 mL/min with detection at 280 nm. The evaluated parameters were specificity, linearity, limits of detection and quantification, precision, accuracy, and robustness. Results: The method was specific and linear (r=0.9982). The limits of detection and quantification were 5.78 μg.mL-1 and 17.54 μg.mL-1, respectively. Suitable accurancy and robustness were obtained. The stability assay showed that pH variation occured after 120 days of storage, and no changes were observed regarding the size and polydispersion parameters. The applicability of the method was evaluated by determining the encapsulation efficiency of the E2 nanocapsules after 120 days of storage. The results showed values >99%. Conclusion: The results demonstrated the applicability of the developed and validated analytical method.

Development and Validation of a High-performance Liquid Chromatography Method with Ultraviolet Detection for the Determination of Flunitrazepam in Human Plasma

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Bela Kiss ◽  
Daniela-Saveta Popa ◽  
Marius Bojita ◽  
Felicia Loghin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Hplc Method ◽  
Simple Liquid ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
The Stability

A high performance liquid chromatography (HPLC) method was developed and validated for determination of flunitrazepam in human plasma. After a simple liquid-liquid extraction, the analyses were carried out on a ODS column with diode array detection at 330nm. The mobile phase consisted in a mixture of potassium dihydrogene phosphate/acetonitrile (40/60, v/v). The method showed good linearity, accuracy and precision. Advantages of this validated assay include a simple plasma extraction method, short analysis time and good sensitivity (LLOQ = 5ng/mL). The stability data indicated a potential instability of flunitrazepam in plasma at room temperature.

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