scholarly journals Separation and Characterization of Novel Degradation and Process Related Impurities of Bedaquiline Bulk Drug

2021 ◽  
Author(s):  
Pragati J Vanavi ◽  
Sadhana J Rajput
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Ultra Performance Liquid Chromatography ◽  
Hplc Method ◽  
Preparative Hplc ◽  
Ionization Mass ◽  
Chromatography Method ◽  
Esi Ms ◽  
Related Impurities

Abstract Bedaquiline (BDQ) is a new drug approved by United States Food and Drug Administration (USFDA) in 2012 for the treatment of drug-resistant tuberculosis, which has become a major threat globally. The manuscript presents the development of three liquid chromatography (LC) based analytical methods. The first is a stability indicating RP-HPLC (reverse phase-high performance liquid chromatography) method to analyze the BDQ in presence of its degradation products. Another UPLC/ESI–MS (ultra-performance liquid chromatography/electron spray ionization–mass spectrometry) method was developed for the identification of different degradation based and process related impurities and the third, preparative HPLC method was developed for the isolation of major degradation products. Eleven degradation products and one process related impurity were identified using UPLC/ESI–MS whereas preparative HPLC was used to isolate two degradation products and their chemical structure was elucidated using nuclear magnetic resonance, mass and infra-red spectral data.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

scholarly journals A NEW HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SEPARATION AND SIMULTANEOUS QUANTIFICATION OF EPTIFIBATIDE AND ITS IMPURITIES IN PHARMACEUTICAL INJECTION FORMULATION

2021 ◽  
pp. 165-172
Author(s):  
K. SRI GIRIJA ◽  
BIKSHAL BABU KASIMALA ◽  
VENKATESWARA RAO ANNA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Ultra Violet ◽  
Hplc Method ◽  
Chromatography Method ◽  
Standard Drug ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard

Objective: The objective of the present study is to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for qualitative and quantitative determination of Eptifibatide and its impurities in bulk and pharmaceutical dosage forms. Methods: The chromatographic separation was carried on Phenomenex Luna C18 column (250 mm×4.6 mm; 5µ id) as stationary phase, methanol and phosphate buffer at pH 6.4 in the ratio of 65:45 (v/v) as mobile phase at flow rate of 1.0 ml/min, Ultra Violet (UV) detection was carried at the wavelength of 236 nm and the analysis was completed with a run time of 15 min. Results: In the developed conditions, the retention time of Eptifibatide and its impurities 1 and 2 were found to be 3.35, 4.93 and 8.18 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50%, 100% and 150% was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for Eptifibatide and both impurities studied and the % Relative standard deviation (RSD) in each spiked level was found to be less than 2. Stability tests were done through the exposure of the analyte solution to five different stress conditions i. e expose to 1N Hydrochloric acid (HCl), 1 N Sodium hydroxide (NaOH), 3% Hydrogen peroxide (H2O2), 80 °C temperature to UV radiation. In all the degradation conditions, standard drug Eptifibatide was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis, there is no other chromatographic detection of other impurities and formulation excipients. Conclusion: The developed method was found to be suitable for the quantification of Eptifibatide and can separate and analyse impurities 1 and 2.

Development and Validation of a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) Method for Identification, Assay and Estimation of Related Substances of Ivermectin in Bulk Drug Batches of Ivermectin Drug Substance

2021 ◽  
Author(s):  
Daoli Zhao ◽  
Rasangi M Wimalasinghe ◽  
Lin Wang ◽  
Abu M Rustum
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Substance ◽  
Related Impurities ◽  
Rp Hplc ◽  
Bulk Drug

Abstract A reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for the identification and assay of Ivermectin, including the identification and estimation of its process-related impurities and degradation products in bulk drug substance of Ivermectin. Analytes were separated on a HALO C18 column (100 mm × 4.6 mm I.D., 2.7 μm particle size) maintained at 40 °C (column temperature) with gradient elution. All analytes of interests were adequately separated within 25 min. All degradation products, process-related impurities and assay were monitored by ultraviolet detection at 254 nm. The new HPLC method described here successfully separated an isomer peak of the active pharmaceutical ingredient (API) from the major API peak. This newly separated isomer peak is around 1.2 to 1.5% (peak area) in typical API samples, and coelutes with the major API peak by all current HPLC methods. Quantitation limit of the HPLC method is 0.1% of target analytical concentration (~1.0 μg/mL). This method has been demonstrated to be accurate, robust, significantly higher degree of selectivity compared to the HPLC methods of Ivermectin drug substance reported in the literature and in the compendial HPLC methods prescribed in the current USA and European Pharmacopeia.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

Profiling and Quantification of the Key Phytochemicals from the Drumstick Tree (Moringa oleifera) and Dietary Supplements by UHPLC-PDA-MS

Planta Medica ◽  
2020 ◽  
Author(s):  
Omer I. Fantoukh ◽  
Yan-Hong Wang ◽  
Abidah Parveen ◽  
Mohammed F. Hawwal ◽  
Gadah A. Al-Hamoud ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Moringa Oleifera ◽  
Negative Ion ◽  
Array Detector ◽  
Ionization Mass ◽  
Fractionation Process ◽  
Chromatography Method ◽  
Drumstick Tree

Abstract Moringa oleifera is known as a drumstick tree and is cultivated in the subtropics and tropics. It exhibits antihypertensive and antidiabetic effects. An ultra-high-performance liquid chromatography method was developed for the determination of 9 phytochemicals in M. oleifera leaves and marketed products. The efficient separation was achieved within 7 min with a temperature of 45 °C by using a C-18 column as the stationary phase and water/acetonitrile with 0.05% formic acid as the mobile phase. The method was validated for linearity, repeatability, limits of detection, and limits of quantification. The limits of detections of phenolic compounds 1 – 9 were as low as 0.2 µg/mL. The photodiode array detector at 220 and 255 nm wavelengths was recruited for quantification. The key phytochemicals were detected in the range of 0.42 to 2.57 mg/100 mg sample weight in 13 dietary supplements. This study considers the quantitative analysis for lignans in M. oleifera for the first time. Isoquercitrin (5) and quercetin 3-O-(6-O-malonyl)-β−D-glucopyranoside (6) predominates the leaves of M. oleifera with inherent degradable nature detected for compound 6. Niazirin (2) was detected in amounts between 0.010 – 0.049 mg/100 mg while compound 1 was undetectable and potentially an artifact because of the fractionation process. The characterization and confirmation of components were achieved by liquid chromatography-electrospray ionization-mass spectrometry with extractive ion monitoring for the positive and negative ion modes. The developed and validated method is robust and rapid in the conclusive quantification of phytochemicals and authentication of the Moringa samples for quality assurance.

DEVELOPMENT AND VALIDATION OF HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF DEXTROMETHORPHAN HYDROBROMIDE AND QUINIDINE SULPHATE IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 35-40
Author(s):  
A. S. Bagde ◽  
V. V. Khanvilkar ◽  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Dextromethorphan Hydrobromide

The present work describes a validated reverse phase high performance liquid chromatography (RPHPLC) method for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate in pharmaceutical dosage from. The drugs were resolved using Hemochrom Intsil C18-5U column (250×4.6) mm in isocratic mode with mobile phase methanol: water (0.08% diethylamine, 0.02% of glacial acetic acid and pH 4.4 adjusted with orthophosphoric acid) in the ratio of 70:30 V/V at a flow rate of 1.0 mL/min. Retention time of dextromethorphan hydrobromide and quinidine sulphate were 4.9±0.2 and 3.6±0.2, respectively, at 292nm. The above mentioned method was validated as per International Conference on Harmonization (ICH) guidelines. Linear responses were obtained in concentration ranges of 5-35 μg/mL for dextromethorphan hydrobromide and 4-16 μg/mL for quinidine sulphate, with correlation coefficient (r2) of 0.999 for both the drugs. A simple, selective, accurate, precise, robust and reliable RP-HPLC method thus developed and validated for simultaneous estimation of dextromethorphan hydrobromide and quinidine sulphate.

Methods for simultaneous determination of 29 legacy and insensitive munition (IM) constituents in aqueous, soil-sediment, and tissue matrices by high-performance liquid chromatography (HPLC)

2021 ◽  
Author(s):  
Bobbi Stromer ◽  
Rebecca Crouch ◽  
Katrinka Wayne ◽  
Ashley Kimble ◽  
Jared Smith ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solvent Extraction ◽  
Environmental Protection Agency ◽  
High Performance ◽  
Solid Phase ◽  
Degradation Products ◽  
Direct Injection ◽  
High Water ◽  
Hplc Method

Standard methods are in place for analysis of 17 legacy munitions compounds and one surrogate in water and soil matrices; however, several insensitive munition (IM) and degradation products are not part of these analytical procedures. This lack could lead to inaccurate determinations of munitions in environmental samples by either not measuring for IM compounds or using methods not designed for IM and other legacy compounds. This work seeks to continue expanding the list of target analytes currently included in the US Environmental Protection Agency (EPA) Method 8330B. This technical report presents three methods capable of detecting 29 legacy, IM, and degradation products in a single High Performance Liquid Chromatography (HPLC) method with either ultraviolet (UV)-visible absorbance detection or mass spectrometric detection. Procedures were developed from previously published works and include the addition of hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX); hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX); hexahydro-1,3,5-trinitroso-1,3,5-triazine (TNX); 2,4-diamino-6-nitrotoluene (2,4-DANT); and 2,6-diamino-4-nitrotoluene (2,6-DANT). One primary analytical method and two secondary (confirmation) methods were developed capable of detecting 29 analytes and two surrogates. Methods for high water concentrations (direct injection), low-level water concentrations (solid phase extraction), soil (solvent extraction), and tissue (solvent extraction) were tested for analyte recovery of the new compounds.

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