Development of an UPLC-MS/MS approach to detect and quantify N-nitroso mirabegron in mirabegron.

In the mirabegron (MIR) synthesis, the N-nitroso mirabegron (NNM) is obtained during synthetic process of MIR; water is being used in reaction under acidic condition. Nitrite source is from water, and secondary amine source is from MIR as it has secondary amine; NNM is generated as an impurity during the synthesis of MIR. The presence of NNM in MIR could potentially affect its effectiveness.

Olaparib Process Development Employing Quality by Design (QbD) Principles.

This study focuses on multivariate experimental design and statistical analysis to optimize the process of Olaparib . Quality by design (QbD) methodology was adopted for optimization of the Olaparib process consisting of three reaction steps: (1) amidation, (2) deprotection, and (3) acylation. Every chemical conversion was studied in isolation, employing risk assessment to identify key material attributes and key process parameters that may have the potential to impact the reaction.

Efficient Process Development of Abiraterone Acetate by Employing Design of Experiments.

This article describes an efficient process for the synthesis of abiraterone acetate by employing Quality by Design (QbD) principles and statistical design of experiments (DoE). It focuses on the identification of critical quality attributes (CQAs), the relationship between CQAs and material attributes (MAs), and critical process parameters (CPPs) for the synthesis of hydrazone, vinyl iodide intermediates, and final product. Risk assessment is employed to identify the probable critical factors involved in each chemical transformation.

CuNi sulphidation maximizes MOR activity by expanding the accessibility of active sites!

Sulphidation of a CuNi alloy of Cu : Ni ratio 81 : 19 led to an exponential activity enhancement in the alkaline methanol oxidation reaction (MOR) by four fold due to an order of magnitude increase in the number of active Cu and Ni sites and improved charge transfer properties.

A tri-functional self-supported electrocatalyst featuring mostly NiTeO perovskite for H production methanol-water co-electrolysis.

A self-supported NiTeO perovskite is made by deploying an extended hydrothermal tellurization strategy with a restricted Te content, which was found to be exceptionally active towards the oxidation of water and methanol and the reduction of water in 1.0 M KOH where it delivered -10 mA cm at just -1.54 V for a full cell featuring MOR‖HER.

RP-LC Method Development and Validation for Dasatinib Forced Degradation Study: Isolation and Structural Characterization by NMR and HRMS.

A reverse phase high-performance liquid chromatography (HPLC) method has been developed for the quantification of a typical drug Dasatinib (DST) and its related impurities in pharmaceuticals. Kinetex C18 (4.6 × 150 mm, 5 μm) column was used in the chromatographic separations, using buffer (1.

Identification of Two Novel Hydroperoxide Impurities in Fluocinolone Acetonide Topical Solution by Liquid Chromatography Mass Spectrometry.

Fluocinolone acetonide topical is used to treat skin discomforts such as swelling, itching and redness by activating the natural substances in the skin. Several process-related impurities and degradation products are identified and reported. But hydroperoxide impurities in Fluocinolone acetonide topical solution are not reported anywhere.

Trace-level determination of potential genotoxic impurities in quetiapine fumarate using LC-MS.

A novel LC-MS method was developed and validated to determine three potential genotoxic impurities, namely 2-(2-aminophenylthio)benzoic acid hydrochloride, 2-aminothiophenol, and 2-(2-aminophenylthio)benzonitrile, at trace level (~1.6 ppm) in quetiapine fumarate drug substance, an antipsychotic drug. These impurities are potentially genotoxic and therefore should be controlled at or below specific acceptance limits.

Hierarchical NaV(PO)F Microsphere Cathodes for High-Temperature Li-Ion Battery Application.

Sodium superionic conductor (NASICON)-structured NaV(PO)F cathode materials have received vast attention in the high-temperature storage performance due to their structural and thermal stability. Herein, hierarchical NaV(PO)F microspheres (NVPF-HMSs) consisting of nanocubes were designed by a one-pot facial solvothermal method. The hierarchical NaV(PO)F microsphere size is 2-3 μm, which is corroborated by FE-SEM and HR-TEM analyses.

A Multi-Analyte LC-MS/MS Method for Determination and Quantification of Six Nitrosamine Impurities in Sartans like Azilsartan, Valsartan, Telmisartan, Olmesartan, Losartan and Irbesartan.

A sensitive and robust method for determination and quantification of potential genotoxic impurities in sartans has been developed. These impurities need to be controlled at trace levels during quantification in drug substances and drug products for safe consumption. Recent regulatory requirements also suggested the need to have highly sensitive analytical method for trace level quantification of nitrosamine impurities.

Recent development on core-shell photo(electro)catalysts for elimination of organic compounds from pharmaceutical wastewater.

Pharmaceutical organics are a vital milestone in contemporary human research since they treat various diseases and improve the quality of human life. However, these organic compounds are considered one of the major environmental hazards after the conception, along with the massive rise in antimicrobial resistance (AMR) in an ecosystem. There are various biological and catalytic technologies existed to eliminate these organics in aqueous system with their limitation.

Stable Fatty Acid Solvates of Dasatinib, a Tyrosine Kinase Inhibitor: Prediction, Process, and Physicochemical Properties.

Exploration of alternate solid forms for dasatinib, a potent oncogene tyrosine kinase inhibitor classified under Biopharmaceutics Classification System (BCS) class II drugs with low water solubility and high permeability, has been performed using COSMO-RS excess enthalpy (Hex) to increase dissolution. The theoretical prediction resulted in the potential for the formation of C-C fatty acid solvates with dasatinib. A crystallization process has been identified for the preparation of the predicted solvates and successfully scaled up till the 100 g level.

Use of Stage-Wise AQbD and an Orthogonality Approach to Develop a Short-Runtime Method for the Simultaneous Quantification of Bosentan and Impurities using UPLC Equipped with PDA and ESI-MS.

Analytical quality by design (AQbD) and method orthogonality are comprehensive tools used to develop an analytical method based on statistical and graphical evaluation. These tools provide complete knowledge of the method and help to develop precise, accurate, and specific methods. The present work elaborates the development of a selective and precise method for the quantification of bosentan and its nine impurities with a short runtime of 10 min using a statistically driven stage-wise AQbD approach with proven orthogonality.

A Stability Indicating Method Development and Validation for Separation of Process Related Impurities and Characterization of Unknown Impurities of Tyrosine Kinase Inhibitor Ibrutinib Using QbD Approach by RP-HPLC, NMR Spectroscopy and ESI-MS.

A selective RP-HPLC method for separation and determination of potential-related impurities (process related and degradants) of Ibrutinib drug substance has been developed and validated. The separation was accomplished on a X-Bridge C18, (150 x 4.6 mm, 3.

Moisture Sorption-desorption Characteristics and the Corresponding Thermodynamic Properties of Carvedilol Phosphate.

Aims: Carvedilol phosphate (CDP) is a nonselective beta-blocker used for the treatment of heart failures and hypertension. In this work, moisture sorption-desorption characteristics and thermodynamic properties of CDP have been investigated.

Materials And Methods: The isotherms were determined using dynamic vapor sorption analyzer at different humidity conditions (0%-90% relative humidity) and three pharmaceutically relevant temperatures (20°C, 30°C, and 40°C).

Physical characterization and dissolution performance assessment of Etravirine solid dispersions prepared by spray drying process.

The aim of the current exertion was to prepare Solid Dispersion of Etravirine by Spray drying technique to enhance aqueous solubility and dissolution rate. Solid dispersions (SD) of Etravirine were prepared using Copovidone and Povidone-Copovidone in dichloromethane and physical properties were characterized by Scanning electron microscopy (SEM), X-Ray diffractometry (PXRD), Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC). SD's were evaluated for equilibrium solubility and in vitro drug release profile by dissolution testing.

Trace Level Quantification of the (-)2-(2-amino-5-chlorophenyl)-4-cyclopropyl-1,1,1-trifluoro-3-butyn-2-ol Genotoxic Impurity in Efavirenz Drug Substance and Drug Product Using LC-MS/MS.

Efavirenz is a non-nucleoside reverse transcriptase inhibitor used in the treatment of human immunodeficiency virus type-1 (HIV). (2S)-(2-Amino-5-chlorophenyl)-4-cyclopropyl-1,1,1-trifluoro-3-butyn-2-ol (AMCOL), used as an intermediate in the synthesis of efavirenz and a degradation impurity, has an aminoaryl derivative which is a well-known alerting function for genotoxic activity. Upon request from a regulatory agency, a selective and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for trace level quantitative determination of AMCOL related compound of efavirenz, for a risk assessment and comparison of impurity levels with the commercially available innovator product (brand name: Sustiva).

Simultaneous estimation of degree of crystallinity in combination drug product of abacavir, lamivudine and neverapine using X-ray powder diffraction technique.

Objective: In the present study, simultaneous determination of degree of crystallinity content in abacavir (ABC), lamivudine (3TC) and neverapine (NVP) from there combination drug product using X-ray powder diffraction (XRPD) technique is developed and validated.

Methods: The X-ray procedure for the identification and determination of the degree of crystallinity in ABC, 3TC and NVP drug product is developed and validated. It is based on the X-ray diffraction from crystalline region of the drug product.