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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 ultra performance liquid chromatography-tandem mass spectrometry method for the simultaneous estimation of dolutegravir, lamivudine and tenofovir in bulk and tablet dosage form

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EUROPEAN JOURNAL OF MASS SPECTROMETRY 2021年第6期27卷 249-255页

作者： Veerareddy, Vyshali dodda, sireesha Gangarapu, Kiran Anurag Univ Dept Pharm Hyderabad India

A simple, selective and rapid ultra performance liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous estimation of dolutegravir, lamivudine and tenofovir in bulk and tablet dosage form. Chromatographic separation was attained on Acquity Ethylene Bridged Hybrid (BEH) C18 column (50 x 2.1 mm, 3.5 mu m), using a mixture of acetonitrile and 0.1% formic acid in water (60:40, v/v) as a mobile phase at a flow rate of 0.12 mL/min. The total run time of analysis was 3.5 min. The analytes were detected using tandem mass spectrometry, operating in positive ionization and multiple reaction monitoring modes. The method's linearity was determined to be in the range of 10-150 ng/mL with r(2) > 0.99. The proposed method was validated as per the International Council for Harmonization (ICH) guidelines, and the results were found well within the acceptance limits. The method was successfully applied for the simultaneous quantification of all the three analytes in the combined tablet dosage form.

关键词： Dolutegravir lamivudine tenofovir ultra performance liquid chromatography-tandem mass spectrometry method development simultaneous estimation

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Simultaneous Bioanalysis of Naproxen and Diphenhydramine in Human Plasma Using Liquid Chromatography-Tandem Mass Spectrometry

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JOURNAL OF APPLIED SPECTROSCOPY 2023年第3期90卷 661-669页

作者： Bezawada, Viritha Mogili, Padma dodda, sireesha Gajula, Ramakrishna Sir CR Reddy Coll Eluru India Andhra Univ Coll Engn Dept Engn Chem Visakhapatnam India Anurag Univ Sch Pharm Hyderabad India VLS Labs Ltd Hyderabad India

A simple, sensitive, and rapid bioanalytical method was developed for the first time for simultaneous estimation of naproxen sodium (NPX) and diphenhydramine hydrochloride (DPH) in human plasma using liquid chromatographytandem mass spectrometry (LC-MS/MS). The isotope-labelled analogs, naproxen 13CD(3) and diphenhydramine D-5 hydrochloric acid, were used as the internal standards. The analytes were extracted from 50 & mu;L of human plasma employing a simple protein precipitation technique. The separation of analytes was carried out on a Zodiac C-18 column (50 x 4.6 mm, 3 & mu;m) using a mixture of HPLC grade acetonitrile and 5 mM ammonium acetate buffer in 0.025% formic acid (60:40, v/v) at a flow rate of 1.0 mL/min. The method showed linearity within the concentration ranges 400 to 120,000 ng/mL for NPX and from 0.80 to 240 ng/mL for DPH with r(2) > 0.99. The method was validated as per the US FDA guidelines and the results were found to be within the acceptance limits. The method was successfully applied for the pharmacokinetic study of both drugs simultaneously after an oral dose of two caplets, each containing NPX 220 mg and DPH 25 mg under fed conditions in human volunteers. Incurred sample reanalysis was also performed to authenticate the reproducibility of the method.

关键词： naproxen diphenhydramine liquid chromatography-tandem mass spectrometry simultaneous bioanalysis pharmacokinetic study

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Bioanalytical method for estimation of procyclidine in human plasma using liquid chromatography-tandem mass spectrometry: Application to pharmacokinetic study

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EUROPEAN JOURNAL OF MASS SPECTROMETRY 2022年第3-4期28卷 89-93页

作者： Bezawada, Viritha Mogili, Padma dodda, sireesha Gajula, Ramakrishna Pallavi Engn Coll Hyderabad Telangana India Andhra Univ Coll Engn Dept Engn Chem Visakhapatnam Andhra Pradesh India Anurag Univ Sch Pharm Hyderabad Telangana India VLS Labs Ltd Hyderabad Telangana India

A rapid, selective and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for quantification of procyclidine hydrochloride in human plasma using Procyclidine D11 hydrochloride as internal standard. Liquid-liquid extraction technique with methyl tertiary butyl ether was used for the extraction of plasma samples. Chromatographic separation of the analyte and the internal standard from the endogenous components was done on Zodiac C-18 column (50 x 4.6 mm, 5 mu m) using a mixture of methanol and 0.1% formic acid in water (70:30, v/v) as mobile phase at a flow rate of 1 mL/min with the run time of 2 min. The detection of the eluents was done using multiple reaction monitoring (MRM) in positive ion mode. Linearity of the method was established in the concentration range of 0.5 to 120 ng/mL. Full validation of the method was done as per USFDA guidelines and the results were well within the acceptance limits. The successful application of the method was done on healthy human subjects under fasting conditions, proving it to be used for bioequivalence and bioavailability (BA/BE) studies of procyclidine.

关键词： procyclidine LC-MS MS bioanalysis liquid-liquid extraction pharmacokinetic study

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Development and validation of bioanalytical liquid chromatography-tandem mass spectrometry method for the estimation of pentoxifylline in human plasma: Application for a comparative pharmacokinetic study

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EUROPEAN JOURNAL OF MASS SPECTROMETRY 2019年第4期25卷 372-380页

作者： dodda, sireesha Makula, Ajitha Polagani, Srinivasa R. Kandhagatla, Raj N. Anurag Grp Inst Dept Pharm Lalitha Coll Pharm Hyderabad India Jawaharlal Nehru Technol Univ IST Dept Pharmaceut Sci Hyderabad India AnaCipher Clin Res Org Hyderabad India Biotech Pharma Hyderabad India

A method for bioanalysis of pentoxifylline in human plasma was developed using liquid chromatography-tandem mass spectrometry, which is simple, specific, and sensitive. Pentoxifylline D5 was used as the internal standard. Employing only 100 mu l of human plasma, processing was done with solid-phase extraction technique. The analyte and the internal standard were separated from endogenous components on Ace phenyl column using a mixture of 5 mM ammonium acetate buffer and high performance liquid chromatography grade acetonitrile (60:40, v/v) as mobile phase at a flow rate of 1 ml/min. The linearity of the method was in the range of 3-1200 ng/ml with r(2) > 0.99. Positive ion MRM mode was used for the detection of the analyte and the internal standard. The method was validated as per the US Food and Drug Administration guidelines and the results were within the acceptance limits. The proposed method was applied for comparative pharmacokinetic study of pentoxifylline after oral administration of 400 and 600 mg tablets to South Indian male subjects under fed conditions.

关键词： Pentoxifylline in human plasma solid-phase extraction liquid chromatography-tandem mass spectrometry comparative pharmacokinetic study incurred sample reanalysis

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Bioanalysis of bedaquiline in human plasma by liquid chromatography-tandem mass spectrometry: Application to pharmacokinetic study

JOURNAL OF MASS SPECTROMETRY AND ADVANCES IN THE CLINICAL LA...

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JOURNAL OF MASS SPECTROMETRY AND ADVANCES IN THE CLINICAL LAB 2024年 31卷 27-32页

作者： Bezawada, Viritha Mogili, Padma Polagani, Srinivasa Rao dodda, sireesha Aurora Degree & PG Coll Hyderabad Telangana India Andhra Univ Coll Engn Dept Chem Engn Visakhapatnam Andhra Pradesh India Anal Lab Pvt Ltd Hyderabad India Anurag Univ Hyderabad India Anurag Univ Ghatkesar 500088 Telangana India

Introduction: A sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for estimation of bedaquiline (BDQ) in human plasma using the deuterated analogue of the analyte, bedaquilined6 (BDQ-d6) as the internal standard. Methods: The plasma sample of 50 mu L was extracted by liquid-liquid extraction using methyl tertiary butyl ether (MTBE). The separation was achieved on Zodiac C18 (50 x 4.6 mm, 5 mu m) column with a mobile phase consisting of methanol and 5 mM ammonium formate in 0.1 % formic acid (w/v) (90:10, v/v) at a flow rate of 1.0 mL/min. Protonated analyte and internal standard were detected on a triple quadrupole mass spectrometer using multiple reaction monitoring (MRM) mode. Results: The linearity of the method was established in the concentration range of 5---1800 ng/mL with correlation coefficient, r2 >= 0.99. All the validated parameters were found well within the limits. Discussion: The method was applied for the first time to evaluate the pharmacokinetic parameters after single oral dose of BDQ 100 mg under fed conditions in healthy human volunteers, and the results were further authenticated by incurred sample reanalysis.

关键词： Bedaquiline LC-MS/MS Bioanalysis Liquid-liquid extraction Pharmacokinetic study Incurred sample reanalysis

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High sensitive LC-MS/MS method for estimation of eluxadoline in human plasma and its application to pharmacokinetic study

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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS 2019年 165卷 65-72页

作者： dodda, sireesha Makula, Ajitha Polagani, Srinivasa Rao Kandhagatla, Raj Narayana Anurag Grp Inst Dept Pharm Hyderabad 500088 India Jawaharlal Nehru Technol Univ Dept pharmaceut Sci IST Hyderabad 500085 India AnaCipher Clin Res Org Hyderabad 500013 India Biotech Pharma Hyderabad 500085 India

A selective, sensitive and high throughput liquid chromatography - tandem mass spectrometry (LC-MS/MS) method was developed and validated for estimation of eluxadoline in human plasma. Plasma samples of analyte with internal standard (eluxadoline13CD3) were extracted using solid phase extraction on Orochem Panthera Deluxe cartridges. Chromatographic separation was performed on Ace Phenyl column (150 x 4.6 mm, 5 mu m), using a mixture of buffer (2 mM ammonium acetate in 0.01% formic acid), acetonitrile and methanol (20:70:10, v/v/v) as mobile phase at a flow rate of 0.8 mL/min. The run time of analyte was 4.0 min. Tandem mass spectrometry, operating in positive ionization and multiple reaction monitoring modes was used for detection of analyte and internal standard. The method was established with a linear dynamic range of 25.0-5000 pg/mL for eluxadoline using 300 mu L human plasma. The sample preparation procedure was consistent and reproducible (accuracy, 96.2-106.1%;precision (%CV), 0.8-6.6%), preventing the ex vivo hydrolysis of acyl glucuronide metabolite of eluxadoline to parent drug. The method was applied successfully to a clinical pharmacokinetic study in six healthy South Indian male subjects under fed conditions and the results were authenticated by incurred sample reanalysis. (C) 2018 Elsevier B.V. All rights reserved.

关键词： Eluxadoline in human plasma Solid phase extraction Liquid chromatography-tandem mass spectrometry Pharmacokinetic studies Incurred sample reanalysis

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A Sensitive and Rapid LC-MS/MS Method for Quantification of Aminocaproic Acid in Human Plasma and its Pharmacokinetic Application

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ANALYTICAL CHEMISTRY LETTERS 2020年第6期10卷 722-731页

作者： Yadlapalli, Siva Sankara Rao Katari, Naresh Kumar dodda, sireesha Surya, Surendra Babu Manabolu GITAM Univ Dept Chem Hyderabad 502329 India Anurag Grp Inst Dept Pharm Hyderabad 500088 India

This paper describes the determination of aminocaproic acid in human plasma by simple, sensitive, and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using aminocaproic D6 acid as the internal standard (ISD). Extraction of aminocaproic acid and ISD was achieved from 200 & mu;L plasma through protein precipitation with acetonitrile. Acetonitrile and 5 mM ammonium acetate buffer in the ratio 60:40 was used as the mobile phase at the flow rate of 1.0 mL/min. The method was developed with a short chromatographic run time of 3.0 min using Ace phenyl column. The retention times of both analyte and ISD were found to be 1.50 & PLUSMN;0.1 min. The quantification of the separated components was done in positive ion mode by Multiple Reaction Monitoring (MRM) with mass transitions from m/z 132.2 (parent ion) to m/z 79.2 (product ion) for aminocaproic acid and from m/z 138.2 (parent ion) to m/z 74.3 (product ion) for the ISD. The method was validated as per the USFDA guidelines. The linearity was established over the concentration range of 0.3-80 & mu;g/ mL with r(2)>0.98. The % recovery was 86.69 % and 98.29 %, respectively for aminocaproic acid and ISD. The inter- and intra- day accuracy and precision (%CV) were in the range of 100.91 to 103.80 % and 0.91 to 3.63 %, respectively. The developed method was successfully applied for pharmacokinetic study in twelve healthy adult male subjects under fasting conditions and the results were authenticated by performing incurred sample reanalysis.

关键词： Aminocaproic acid LC-MS MS bioanalysis pharmacokinetic study human plasma validation

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Development and validation of bioanalytical method for quantification of cycloserine in human plasma by liquid chromatography-tandem mass spectrometry: Application to pharmacokinetic study

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BIOMEDICAL CHROMATOGRAPHY 2019年第8期33卷 e4548-e4548页

作者： dodda, sireesha Makula, Ajitha Kandhagatla, Raj Narayana Anurag Grp Inst Dept Pharm Hyderabad Telangana India Jawaharlal Nehru Technol Univ Dept pharmaceut Sci IST Hyderabad Telangana India Biotech Pharma Hyderabad Telangana India

A selective, sensitive and high-throughput liquid chromatography-tandem mass spectrometry bioanalytical method has been developed for the estimation of cycloserine in human plasma, employing cytosine as the internal standard. The extraction of the analyte was facilitated by solid-phase extraction using 100 mu L of human plasma. The separation was carried out on a BDS Hypersil C-18 (150 x 4.6 mm, 5 mu m) column using a mixture of 0.2% formic acid in HPLC-grade water, methanol and acetonitrile (70:15:15, v/v/v) as mobile phase at a flow rate of 1.0 mL/min. The method was linear over the range of 0.20-20 mu g/mL with r(2) > 0.99. Complete validation of the method was performed as per US Food and Drug Administration guidelines and the results met acceptance criteria. Applying the present method, the clinical pharmacokinetics of cycloserine following oral administration of 250 mg cycloserine was studied under fasting conditions. Assay reproducibility was also verified by incurred sample reanalysis.

关键词： bioanalysis cycloserine LC-MS MS pharmacokinetic study solid-phase extraction

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Bioanalysis of trifluoperazine in human plasma by LC-MS/MS: Application to disposition kinetics

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BIOMEDICAL CHROMATOGRAPHY 2022年第12期36卷 e5499页

作者： Bezawada, Viritha Mogili, Padma dodda, sireesha Gajula, Ramakrishna Ponnada, Suhasini Aurora Degree & PG Coll Hyderabad Telangana India Andhra Univ Coll Engn Dept Engn Chem Visakhapatnam Andhra Pradesh India Anurag Univ Hyderabad India VLS Clin Res Org Hyderabad Telangana India Aurobindo Pharma Ltd Hyderabad Telangana India

A sensitive, selective and rapid bioanalytical method using liquid chromatography-tandem mass spectrometry has been developed for the quantification of trifluoperazine in human plasma. Trifluoperazine-D-8 was used as the internal standard and the extraction from human plasma was performed by liquid-liquid extraction technique using tertiary butyl methyl ether as the solvent. Chromatographic separation was carried out on Zodiac C-18 column (50 x 4.6 mm, 3 mu m) employing a mixture of acetonitrile, methanol and 5 mm ammonium bicarbonate buffer in water (85:10:5, v/v/v) at a flow rate of 0.55 ml/min. The linearity was established within the concentration range of 5-1,250 pg/ml with r(2) > 0.99. The results of all of the validation parameters as per the US Food and Drug Administration guidelines were within the acceptance limits. The pharmacokinetics of trifluoperazine after oral administration of a syrup of 1 mg dose under fasting conditions was determined by successful application of the present method.

关键词： bioanalysis LC-MS MS liquid-liquid extraction pharmacokinetic study trifluoperazine

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