Data · dataset · 2026
A sensitive LC-MS/MS method for quantification and conformer resolution of N-nitroso cinacalcet in cinacalcet drug products
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<p>Nitrosamine drug substance-related impurities (NDSRIs) are a cohort of concern due to their potential mutagenic and carcinogenic effects.
Description
Strict guidelines from regulatory authorities have been implemented for their identification and quantification in pharmaceutical formulations to reduce health-related risks. N-Nitroso cinacalcet (NCIN), which is a type of high-risk NDSRI related to cinacalcet is classified under potency class three by United States food and drug administration (USFDA) having daily intake limit of 400 ng/day.
In this study, an liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of NCIN in cinacalcet tablet formulations. Chromatographic separation was achieved on an Eclipse Plus C18 RRHD column (100 × 2.1 mm, 1.8 µm) using a gradient elution program consisting of 10 mM ammonium acetate buffer (pH 3.8, adjusted with 0.1% formic acid) and methanol at a flow rate of 0.4 mL/min.
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Under the optimized conditions, NCIN was resolved into two chromatographic peaks at retention times of 11.86 and 12.39 min, corresponding to anti and syn conformational isomers generated by restricted rotation around the nitrosamine N–N bond. The method exhibited excellent linearity (r<sup>2</sup> > 0.99) over 1–200 ng/mL with limit of detection (LOD) and limit of quantification (LOQ) values of 0.5 and 1.0 ng/mL, respectively, demonstrating suitability for regulatory compliance and pharmaceutical safety monitoring.</p> <p>Workflow for the determination of N-nitroso cinacalcet (NCIN), a nitrosamine impurity, in cinacalcet tablets.
The workflow illustrates potential NCIN formation, preparation of tablet samples, LC-MS/MS analysis, and detection of NCIN by multiple reaction monitoring (MRM) with the resulting chromatographic response.</p>
Links
Where it is published
- DOI doi.org/10.6084/m9.figshare.34023749.v1 ↗
DOI / persistent id · from zivahub uct ac za
Catalogue records · 1
- OAI-PMH record api.figshare.com/v2/oai?verb=GetRecord&metadataPrefix=oai_dc&identifier=oai%3Af… ↗
metadata API · from zivahub uct ac za
Topics
- From keywords
- Biochemistry and cell biology · Chemistry · Earth & Environmental Science · Immunology · Life Sciences · Mass spectrometry · Medicine & Health
Provenance · 1 source records, 12 field assertions
| Source | Key | Last seen | Raw |
|---|---|---|---|
| ZivaHub | oai:figshare.com:article/34023749 | 9 d ago | JSON v1 |
| Field | Assertion | Extractor | Evidence |
|---|---|---|---|
| access_level | source · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | |
| concepts[field].anzsrc:group:3101 | mapping · zivahub uct ac za | vocabulary-mapper@1.0.0 | keywords['Cell Biology'] |
| concepts[field].anzsrc:group:3204 | mapping · zivahub uct ac za | vocabulary-mapper@1.0.0 | keywords['Immunology'] |
| concepts[field].local:field:chemistry | mapping · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | |
| concepts[field].local:field:earth-environmental | mapping · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | |
| concepts[field].local:field:life-sciences | mapping · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | |
| concepts[field].local:field:medicine-health | mapping · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | |
| concepts[modality].local:modality:mass-spectrometry | mapping · zivahub uct ac za | vocabulary-mapper@1.0.0 | keywords['LC-MS/MS'] |
| description | source · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | /metadata/dc/description |
| license | source · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | /metadata/dc/rights |
| publication_date | source · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | |
| title | source · zivahub uct ac za | connector:zivahub_uct_ac_za@1.0.0 | /metadata/dc/title |