Online large volume sample staking preconcentration and separation of enantiomeric GHRH analogs by capillary electrophoresis.
capillary electrophoresis
doping
electrokinetic preconcentration
enantioseparation
peptide
Journal
Electrophoresis
ISSN: 1522-2683
Titre abrégé: Electrophoresis
Pays: Germany
ID NLM: 8204476
Informations de publication
Date de publication:
05 2023
05 2023
Historique:
revised:
20
01
2023
received:
28
11
2022
accepted:
04
02
2023
medline:
12
5
2023
pubmed:
15
2
2023
entrez:
14
2
2023
Statut:
ppublish
Résumé
A capillary electrophoresis method is proposed to analyze the four most well-known growth hormone-releasing hormone (GHRH) analogs that are misused by athletes. Dimethyl-β-cyclodextrin used as a chiral selector allowed, for the first time, the separation of those basic peptide analogs, including enantiopeptides (sermorelin and CJC-1293) that differ by the chirality of only one amino acid. To increase the method sensitivity, electrokinetic preconcentration methods have been investigated. The large volume sample stacking with polarity switching (PS-LVSS) method with an injected sample volume corresponding to 80% of the capillary one was found superior to the sweeping in terms of signal enhancement factor (SEF). Acid and organic solvent addition to the sample (0.1 mM phosphoric acid with 30% methanol) led to a twofold signal improvement, when compared to water as a matrix. We increased capillary dimensions to provide a signal enhancement through the injection of a larger sample volume. Finally, using a combination of the optimized PS-LVSS preconcentration with the chiral capillary zone electrophoresis (CZE), the GHRH analogs were separated and limits of detection between 75 and 200 ng/mL were reached. This method was successfully applied to urine after a desalting step. An optimized C18 SPE was used for that purpose in order to provide low sample conductivity (<130 µS/cm) and preserve the efficiency of LVSS preconcentration. SEF of 640 was obtained with desalted urine spiked with sermorelin by comparison to the CZE (without preconcentration) method.
Identifiants
pubmed: 36787346
doi: 10.1002/elps.202200278
doi:
Substances chimiques
Sermorelin
86168-78-7
Solvents
0
Methanol
Y4S76JWI15
Growth Hormone-Releasing Hormone
9034-39-3
Types de publication
Journal Article
Research Support, Non-U.S. Gov't
Langues
eng
Sous-ensembles de citation
IM
Pagination
807-817Informations de copyright
© 2023 The Authors. Electrophoresis published by Wiley-VCH GmbH.
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