NMR Reveals an Undeclared Constituent in Custom Synthetic Peptides
| العنوان: | NMR Reveals an Undeclared Constituent in Custom Synthetic Peptides |
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| المؤلفون: | Mary P. Choules, JB McAlpine, Charlotte Simmler, Matthias Niemitz, Anton Bzhelyansky, Jonathan Bisson, Guido F. Pauli, Gabriel I. Giancaspro |
| المساهمون: | Groupe d’Etudes des Substances Végétales à Activité Biologique (GESVAB ), Thallion Pharmaceuticals Inc. |
| المصدر: | J Pharm Biomed Anal Journal of Pharmaceutical and Biomedical Analysis Journal of Pharmaceutical and Biomedical Analysis, Elsevier, 2020, 178, pp.112915. ⟨10.1016/j.jpba.2019.112915⟩ Journal of Pharmaceutical and Biomedical Analysis, 2020, 178, pp.112915. ⟨10.1016/j.jpba.2019.112915⟩ |
| سنة النشر: | 2019 |
| مصطلحات موضوعية: | Adulterant, Quality Control, 010405 organic chemistry, Chemistry, Clinical Biochemistry, Pharmaceutical Science, 010402 general chemistry, 01 natural sciences, Magnetic Resonance Imaging, Article, 0104 chemical sciences, Analytical Chemistry, Custom peptide synthesis, Pharmaceutical Preparations, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Drug Discovery, Biochemical engineering, Drug Contamination, Peptides, Spectroscopy, ComputingMilieux_MISCELLANEOUS |
| الوصف: | Whereas generic, LC-based pharmaceutical control quality procedures depend largely on the detection mode and can be particularly ‘blind’ to certain impurities, NMR is a more versatile and, thus, often more judicious detector. While adulteration presents ever-evolving challenges for the analysis of active pharmaceutical ingredients (APIs) and finished products sold in the worldwide (online) marketplace, research chemicals are usually trusted rather than being considered flawed or even adulterated. This report shows how NMR analysis uncovered the unanticipated presence of substantial amounts of mannitol (20 and 43% w/w) as undeclared constituent in two custom synthetic peptides, DR and DRVYI, that were sourced commercially. Quantitative 1H NMR (qHNMR) readily detected the contaminant, even on a 60 MHz benchtop instrument, and quantified the highly polar and UV-transparent adulterant. Quantum-mechanical 1H iterative Full Spin Analysis (HiFSA) not only achieved unambiguous identification of both the mannitol and the peptides, but also confirmed the quantitative results. The cases show that experimental verification supersedes trust in both pharmaceutical and research QC. They also highlight the promising utility of both established high-field and recently re-evolving low-field benchtop qHNMR. The unanticipated findings remind manufacturers and researchers alike about the advantages of including/performing NMR and qNMR with routine CofA documentation and/or verification of research grade chemicals. Especially when done jointly, this can greatly improve confidence in research and help streamline the pharmaceutical QC toolbox. |
| اللغة: | English |
| تدمد: | 0731-7085 1873-264X |
| DOI: | 10.1016/j.jpba.2019.112915⟩ |
| URL الوصول: | https://explore.openaire.eu/search/publication?articleId=doi_dedup___::bb4f5df7fd07c1f2967cf9d82986bfcd https://europepmc.org/articles/PMC6913887/ |
| Rights: | OPEN |
| رقم الانضمام: | edsair.doi.dedup.....bb4f5df7fd07c1f2967cf9d82986bfcd |
| قاعدة البيانات: | OpenAIRE |
| تدمد: | 07317085 1873264X |
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| DOI: | 10.1016/j.jpba.2019.112915⟩ |