From Targeted LC-MS/MS to High-Resolution Mass Spectrometry: Emerging Analytical Strategies for the Characterization of Antiviral and Antibacterial Drugs, Impurities and Degradation Products: A Critical Review

Authors

  • Niloufer Tasnim Khazi Department of Pharmacy, Chaitanya Deemed to be University, Gandipet, Hyderabad 500075, Telangana, India
  • Kumara Swamy Gandla Department of Pharmacy, Chaitanya Deemed to be University, Gandipet, Hyderabad 500075, Telangana, India

DOI:

https://doi.org/10.68163/ptr.2026.68

Keywords:

Antibacterial drugs, antiviral drugs, degradation products, forced degradation, high-resolution mass spectrometry, impurities, LC-MS/MS, orbitrap, pharmaceutical analysis, QTOF, UHPLC, UPLC-MS/MS

Abstract

Antiviral and antibacterial medicines present a particularly broad analytical challenge. The same laboratory may need to quantify a known impurity at trace levels, investigate an unexpected peak arising during stability studies and distinguish a genuine degradation product from an adduct, isomer, or source-generated fragment. Targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS), particularly triple-quadrupole multiple-reaction monitoring (MRM), remains highly effective for the sensitive and selective quantification of predefined analytes. In contrast, high-resolution mass spectrometry (HRMS) provides complementary capabilities through accurate-mass full-scan measurements and product-ion data, which can be interrogated when the composition of an impurity is not known in advance. This review examines how these complementary capabilities can be integrated into the analysis of antiviral and antibacterial drug substances and pharmaceutical products. Recent studies published between 2022 and 2026 are considered alongside established analytical principles, with particular emphasis on forced degradation, impurity origin, chromatographic selectivity, ionization behaviour, fragmentation evidence, isomeric ambiguity, matrix effects and the level of evidence required to support structural assignments. Recent examples in antiviral drug analysis include Maillard-reaction impurities of acyclic nucleoside analogues, forced-degradation products of darunavir, impurities of peramivir, bictegravir-related substances and degradation products of umifenovir. An example from antibacterial drug analysis is the LC-HRMS/MS characterization of dalbavancin degradation products. Collectively, these studies demonstrate that accurate-mass measurements are most informative when interpreted in conjunction with retention behaviour, dependence on stress conditions, isotope patterns, product-ion shifts and , where necessary, reference standards or orthogonal structural characterization techniques. Accordingly, this review considers targeted LC-MS/MS and LC-HRMS as complementary components of a fit-for-purpose analytical workflow rather than as competing platforms. The current principles outlined in ICH Q2(R2) and Q14 are also considered in the context of analytical procedure performance and lifecycle development. Emerging approaches, including data-independent acquisition, ion mobility spectrometry and computational spectral annotation, are discussed cautiously as complementary tools that may strengthen, rather than replace, expert interpretation. Overall, the available evidence supports an integrated analytical strategy in which HRMS is primarily employed to elucidate chemical identity and targeted LC-MS/MS is applied when sensitive, selective and robust routine quantification is required.

References

Narayanam M, Handa T, Sharma P, Jhajra S, Muthe PK, Dappili PK et al. Critical practical aspects in the application of liquid chromatography–mass spectrometric studies for the characterization of impurities and degradation products. J Pharm Biomed Anal. 2014;87:191-217.

Beccaria M, Cabooter D. Current developments in LC-MS for pharmaceutical analysis. Analyst. 2020;145(4):1129-1157.

Khalikova M, Jireš J, Horáček O, Douša M, Kučera R, Nováková L. What is the role of current mass spectrometry in pharmaceutical analysis? Mass Spectrom Rev. 2023;43(3):560-609.

Lai X, Chen X, Li M, Zhou Y, Xia B. Purification and mass spectrometry study of Maillard reaction impurities in five acyclic nucleoside antiviral drugs. J Pharm Biomed Anal. [Internet]. 2022;212. Available from: https://doi.org/10.1016/j.jpba.2022.114637

Modini AK, Ranga M, Puppala U, Kaliyapermal M, Geereddy MKR, Samineni R et al. Identification, isolation, and structural characterization of novel forced degradation products of darunavir using advanced analytical techniques like UPLC–MS, Prep-HPLC, HRMS, NMR, and FT-IR spectroscopy. Chromatographia. 2022;86:63-78.

Alumuri T, Merugu KS, Namburi LAA, Kurnool A, SaravanaVadivu A, Balasubramanian S. An antiviral drug—peramivir: Degradation and identification of impurities and the endorsement of an HPLC–MS method. J AOAC Int. 2023;106(5):1138-1144.

Kumar SRJ, Rao VK, Katari NK, Jyothi NS, Kowtharapu LP. Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry. Anal Methods. 2023;15(10):1274-1285.

Paritala ST, Sharma N, Shah RP. A comprehensive study on the identification and characterization of degradation products of lipoglycopeptide dalbavancin using LC and LC-HRMS/MS. J Pept Sci. [Internet]. 2024;30(10). Available from: https://doi.org/10.1002/psc.3608

Kaufmann A. The current role of high-resolution mass spectrometry in food analysis. Anal Bioanal Chem. 2011;403:1233-1249.

International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. Validation of analytical procedures. Q2(R2). ICH Harmonised Guideline. International Council for Harmonisation; 2023. https://database.ich.org/sites/default/files/ICH_Q2%28R2%29_Guideline_2023_1130.pdf

International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. Analytical procedure development. Q14. ICH Harmonised Guideline. International Council for Harmonisation; 2023. https://database.ich.org/sites/default/files/ICH_Q14_Guideline_2023_1116.pdf

Niessen WMA. Tandem mass spectrometry of small-molecule antiviral drugs: 1. HIV-related antivirals. Int J Mass Spectrom. [Internet]. 2020;455. Available from: https://doi.org/10.1016/j.ijms.2020.116370

Schymanski EL, Jeon J, Gulde R, Fenner K, Ruff M, Singer HP et al. Identifying small molecules via high resolution mass spectrometry: Communicating confidence. Environ Sci Technol. 2014;48(4):2097-2098.

Blessy M, Patel RD, Prajapati PN, Agrawal YK. Development of forced degradation and stability indicating studies of drugs—A review. J Pharm Anal. 2014;4(3):159-165.

Matuszewski BK, Constanzer ML, Chavez-Eng CM. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC−MS/MS. Anal Chem. 2003;75(13):3019-3030.

Ramakrishnan B, Raju JM, Thangavelu P, Mariappan E, Natarajan J, Selvaraj J. Significance of impurity analysis in antiviral drug: A critical review. Curr Drug Res Revs. 2025;17(3):394-411.

Somkuwar K, Sabale P, Sawale V, Ikhar R, Sabale V. Identification, separation of stress degradation impurities of antiviral drug umifenovir by UFLC and their structural elucidation using hyphenated technique LC-HRMS. Anal Chem Lett. 2026;16(2):131-147.

Cordeiro CF, Franco LL, Carvalho DT, Bonfilio R. Impurities in active pharmaceutical ingredients and drug products: A critical review. Crit Revs Anal Chem. 2024;56(1):55-75.

Rambhad SR, Dave H. A review on applications of liquid chromatography coupled with mass spectrometry in impurity profiling of drug substances and drug products. SepSci Plus. [Internet]. 2025;8(6). Available from: https://doi.org/10.1002/sscp.70073

Broadhurst D, Goodacre R, Reinke SN, Kuligowski J, Wilson ID, Lewis MR et al. Guidelines and considerations for the use of system suitability and quality control samples in mass spectrometry assays applied in untargeted clinical metabolomic studies. Metabolomics. [Internet]. 2018;14. Available from: https://doi.org/10.1007/s11306-018-1367-3

Broeckling CD, Beger RD, Cheng LL, Cumeras R, Cuthbertson DJ, Dasari S et al. Current practices in LC-MS untargeted metabolomics: A scoping review on the use of pooled quality control samples. Anal Chem. 2023;95(51):18645-18654.

International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. Impurities in new drug substances. Q3A(R2). ICH Harmonised Tripartite Guideline. International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use; 2006. https://database.ich.org/sites/default/files/Q3A%28R2%29%20Guideline.pdf

International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. Impurities in new drug products. Q3B(R2). Current Step 4 version. International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use; 2006. https://database.ich.org/sites/default/files/Q3B%28R2%29%20Guideline.pdf

International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. Application of the principles of the ICH M7 guideline to calculation of compound-specific acceptable intakes. Addendum to M7(R2). Final version. International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use; 2023. https://database.ich.org/sites/default/files/ICH_M7%28R2%29_Addendum_Step4_2023_0216_0.pdf

Kartowikromo KY, Olajide OE, Hamid AM. Collision cross section measurement and prediction methods in omics. J Mass Spectrom. [Internet]. 2023;58(9). Available from: https://doi.org/10.1002/jms.4973

Xia J, Jin Y, Hong Y, Huang X, Pan J, Sun K et al. Application of advanced high‐resolution mass spectrometric techniques for the analysis of losartan potassium drug substance degradation products: From nontargeted to targeted screening. J Sep Sci. [Internet]. 2024;47(23). Available from: https://doi.org/10.1002/jssc.70027

Downloads

Published

2026-09-09

Issue

Section

Review

How to Cite

1.
Khazi NT, Gandla KS. From Targeted LC-MS/MS to High-Resolution Mass Spectrometry: Emerging Analytical Strategies for the Characterization of Antiviral and Antibacterial Drugs, Impurities and Degradation Products: A Critical Review. Pharmacol. Toxicol. Res. [Internet]. 2026 Sep. 9 [cited 2026 Sep. 9];2:41–54. Available from: https://acadpub.com/ptr/article/view/lc-ms-ms-high-resolution-mass-spectrometry-antiviral-antibacterial-drugs-impurities-degradation-products