An effective validation of analytical method for determination of a polar complexing agent: the illustrative case of cytotoxic bleomycin.
Biological
Liquid chromatography
Mass spectrometry
Measurement uncertainty
Pharmaceutical
Stability
Journal
Analytical and bioanalytical chemistry
ISSN: 1618-2650
Titre abrégé: Anal Bioanal Chem
Pays: Germany
ID NLM: 101134327
Informations de publication
Date de publication:
Jun 2023
Jun 2023
Historique:
received:
05
01
2023
accepted:
28
03
2023
revised:
02
03
2023
medline:
17
5
2023
pubmed:
12
4
2023
entrez:
11
4
2023
Statut:
ppublish
Résumé
The effectiveness of highly polar agents in cancer treatment is well recognized, but their physicochemical properties make their analytical determination a demanding task. Their analysis requires peculiar sample preparation and chromatographic separation, which heavily impacts the precision of such an analytical method. As a case study, we chose a polar cytotoxic bleomycin, which is a mixture of complexing congeners with relatively high molecular mass, a fact that creates an added challenge in regard to its detection via electrospray mass spectrometry. These issues combined lead to a deprived method performance, so the aim of this study is manifold, i.e., to optimize, validate, and establish quality performance measures for determination of bleomycin in pharmaceutical and biological specimens. Quantification of bleomycin is done at diametrically different concentration levels: at the concentrations relevant for analysis of pharmaceutical dosage forms it is based on a direct reversed-phase HPLC-UV detection, involving minimum sample pretreatment. On the contrary, analysis of bleomycin in biological specimens requires phospholipid removal and protein precipitation followed by HILIC chromatography with MS/MS detection of bleomycin A2 and B2 copper complexes being the predominant species. This study further attempts to solve the traceability issue in the absence of certified reference standards, determines measurement uncertainty, investigates BLM stability and method performance characteristics, and, last but not least, provides an explanatory example of how a method quality assurance procedure should be established in case of an exceedingly complex analytical method.
Identifiants
pubmed: 37041279
doi: 10.1007/s00216-023-04675-x
pii: 10.1007/s00216-023-04675-x
pmc: PMC10185589
doi:
Substances chimiques
Bleomycin
11056-06-7
Antineoplastic Agents
0
Pharmaceutical Preparations
0
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
2737-2748Subventions
Organisme : Slovenian Research Agency
ID : J1-6744
Organisme : Slovenian Research Agency
ID : J3-9269
Organisme : Slovenian Research Agency
ID : J4-2546
Organisme : Slovenian Research Agency
ID : P1-0143
Informations de copyright
© 2023. The Author(s).
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