Development and validation of rapid ultra high performance liquid chromatography with tandem mass spectroscopic method for the quantification of N-nitrosodimethyl amine and N-nitrosodiethyl amine in sitagliptin and metformin hydrochloride immediate and extended-release formulations.
mass spectrometry
metformin
nitrosamines
sitagliptin
ultra high performance liquid chromatography
Journal
Journal of separation science
ISSN: 1615-9314
Titre abrégé: J Sep Sci
Pays: Germany
ID NLM: 101088554
Informations de publication
Date de publication:
Aug 2022
Aug 2022
Historique:
revised:
20
06
2022
received:
16
03
2022
accepted:
26
06
2022
pubmed:
1
7
2022
medline:
31
8
2022
entrez:
30
6
2022
Statut:
ppublish
Résumé
A simple, effective LC-MS based method is developed and validated to determine N-nitrosodimethylamine and N-nitrosodiethylamine in pharmaceutical formulations of Sitagliptin and Metformin hydrochloride combination dosage forms. Atlantis T3 (100 × 3 mm, 3 μm) column, eluent-A (0.1% formic acid in water), and eluent-B (0.1% formic acid in methanol) were used to achieve chromatographic separation. A gradient program time (min)/%B: 0.01/3, 2/3, 4/55, 5/55, 5.5/90, 6.0/90, 6.5/3, and 7/3, and column flow rate: 0.75 mL/min was employed. The column oven and auto sample cooler temperatures were 40°C and 10°C, respectively. Atmospheric Pressure Ionisation positive mode with corona discharge potential as 4.0 V, drying gas (N
Identifiants
pubmed: 35771715
doi: 10.1002/jssc.202200226
doi:
Substances chimiques
Amines
0
Metformin
9100L32L2N
Sitagliptin Phosphate
TS63EW8X6F
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
3067-3081Informations de copyright
© 2022 Wiley-VCH GmbH.
Références
ICH guideline M7(R1) on assessment and control of DNA reactive (mutagenic) impurities in pharmaceuticals to limit potential carcinogenic risk, ICH M7, 2018.
https://www.fda.gov/drugs/drug-safety-and-availability/information-about-nitrosamine-impurities-medications “Information about Nitrosamine Impurities in Medications”
https://www.ema.europa.eu/en/human-regulatory/post-authorisation/referral-procedures/nitrosamine-impurities “Nitrosamine impurities”
USFDA released guidance on “Control of Nitrosamine Impurities in Human Drugs”(last time accessed: February 2021).
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