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Identification and characterization of unknown oxidation degradation products of Rimegepant by HPLC and triple quadrupole mass spectrometry

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EUROPEAN JOURNAL OF MASS SPECTROMETRY 2025年第1-2期31卷 38-50页

作者： Godi, Narayana reddy Dodda, Sireesha vanga, nagavardhana reddy Ummiti, Kumarswamy Anurag Univ Sch Pharm Dept Pharmaceut Anal Hyderabad 500088 Telangana India GITAM Deemed Be Univ Ind Chem Prod Dev & Anal Ctr GITAM Sch Sci Dept Chem Bengaluru Campus Bengaluru Karnataka India Koneru Lakshmaiah Educ Fdn Coll Engn Dept Chem Guntur Andhra Pradesh India

Rimegepant is a calcitonin gene-related peptide receptor antagonist that has been licensed for migraine headache treatment in the United States, the European Union, the United Kingdom, Hong Kong, Australia, and Kuwait. The oxidation stress study of the Rimegepant drug substance revealed the presence of five impurities. Rimegepant degraded by 5% under the selected oxidation conditions, meeting regulatory expectations. Four out of five impurities are enhanced by more than 1%. This research aims to characterize these oxidation degradation products utilizing the triple quadrupole mass spectroscopic technique. The Rimegepant oxidation degradation products were identified using an optimized chromatographic method that relies on reverse-phase HPLC with PDA detection. This technique utilized a Waters Xbridge C18 column with an eluent mixture of acetonitrile and 0.1% formic acid in water. The oxidation products of Rimegepant have been effectively separated, with a resolution above 3.0. Triple quadrupole mass spectrometry analysis characterized the five degradation products, which showed three N-oxide impurities with masses m/z 566, m/z 550, and m/z 548, as well as two hydrolysis products with masses, m/z 218, m/z 290. These new impurities deserve special attention because the drug's potency and related impurity levels determine any pharmaceutical medication product's quality, safety, and effectiveness.

关键词： Rimegepant oxidation stress study degradation products HPLC TQ-MS

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Development and Validation of a Method for Trace Level Zinc Quantification in Pharmaceutical Zinc Supplements Using a Carboxyl Functional Group Packed Column and Refractive Index Detector

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JOURNAL OF AOAC INTERNATIONAL 2024年第1期107卷 2-13页

作者： vanga, nagavardhana reddy Kesamsetty, Venkata Ratnam Ummiti, Kumaraswamy Ratnakaram, Venkata Nadh Bapatu, Hanimi reddy GITAM Deemed Be Univ Ind Chem Prod Dev & Anal Ctr Dept Chem GITAM Sch Sci Bengaluru Campus Bengaluru 561203 Karnataka India Koneru Lakshmaiah Educ Fdn Dept Chem Coll Engn Guntur 522502 Andhra Pradesh India JNT Univ Dept Chem Hyderabad 500085 Telangana India

Background: Zinc helps with cell division, growth, wound healing, and carbohydrate breakdown. Humanbeings have to obtain zinc from food or supplements because our bodies do not produce it naturally. In view of the greater advantages (such as low cost, time of analysis, and stability-indicating) compared to other quantification methods (titration, ion chromatography, Atomic absorption spectroscopy) proposed in the literature, a refractive index detector coupled with HPLC has been used in quantification of zinc. Objective: The goal of this research is to develop and validate a sensitive, low-cost, high-resolution, and stability- indicating method for detecting and quantifying zinc levels in zinc supplement pharmaceutical products (injectables, tablets, and capsules). Methods: A novel isocratic reverse-phase HPLC method with a refractive index detector (with sensitivity 64, detector temperature 35 degrees C, and positive polarity) was developed using a carboxyl functional group packed column and 0.8% (v/v) formic acid as the mobile phase to detect and quantify zinc content. Results: The reported method has a good optimal sensitivity (LOQ: 0.006 mg/mL and LOD: 0.002 mg/mL). The correlation coefficient (r) obtained from the zinc calibration plot was greater than 0.998, indicating that the method was linear and that there was a strong correlation between zinc concentration (0.006 mg/mL to 0.375 mg/mL) and peak response. The accuracy at LOQ level was found to be 95-105% and 97-103% at the remaining levels (50%, 100%, and 150%). Conclusion: The proposed method was successfully developed and validated as per International council for harmonisation (ICH) guidelines. Therefore, this method can be used for the quantitative testing of zinc in the QC laboratory.

关键词： Refractive index

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Development of a Stability-Indicating Purity Method for Ubrogepant Through Stress Degradation Analysis, Extraction, and Characterization of Unidentified Degradation Products Using Flash Chromatography, NMR, IR, and LC-MS

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JOURNAL OF AOAC INTERNATIONAL 2024年第5期107卷 761-773页

作者： vanga, nagavardhana reddy Ratnam, K. Venkata Ummiti, Kumarswamy Ratnakaram, Venkata Nadh GITAM Deemed Univ Ind Chem Prod Dev & Anal Ctr Dept Chem Bengaluru Campus Bengaluru 561203 Karnataka India Koneru Lakshmaiah Educ Fdn Coll Engn Dept Chem Guntur 522502 Andhra Pradesh India

Background Ubrogepant is a prescription medication used to prevent migraine headaches. It is currently available in tablet *** The goal of this work is to investigate the drug degradation profile of ubrogepant, as well as to isolate and characterize undiscovered ubrogepant degradation products by utilizing LC-MS, NMR, and IR spectroscopic analytical techniques and, furthermore, to develop a high-resolution, sensitive, stability-indicating analytical approach for detecting and quantifying ubrogepant degradation products in its pharmaceutical *** To identify and quantify the degradation products of ubrogepant in pharmaceutical products, a novel gradient reverse-phase HPLC (RP-HPLC) technique with a photo diode array (PDA) detector was developed by utilizing a C18 stationary phase column. The eluent comprised a mixture of acetonitrile and water with 0.1% (v/v) ortho-phosphoric acid. To establish the intrinsic stability of the ubrogepant pharmaceutical product, it was stress-tested under various degradation conditions, including water, alkaline, acid hydrolysis, photolytic, oxidative, and thermal. Flash chromatography was used to isolate the two major degradants, and the structures were determined using NMR (1H, 13C, distortionless enhancement by polarisation transfer-DEPT-135), IR, and LC-MS *** The ubrogepant medication was relatively more degradable in alkaline and acidic conditions, and two unique degradation products were discovered. Based on spectroscopic and chromatographic evidence, it was conclusively demonstrated that these unique compounds were ubrogepant hydrolysis products. All degradation products were separated with a resolution greater than 2.0. The peak purity data showed that the ubrogepant peak in all of the stress samples examined was pure. Under all stress environments, ubrogepant achieved a minimum mass balance of 95%. The validated approach developed was sensitive enough to quantify ubrogepant degradation pro

关键词： Hydrolysis

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