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  • Simultaneous analysis of vitamins B in pharmaceuticals and dietary supplements by capillary electrophoresis hyphenated with triple quadrupole mass spectrometry.

Simultaneous analysis of vitamins B in pharmaceuticals and dietary supplements by capillary electrophoresis hyphenated with triple quadrupole mass spectrometry.

Die Pharmazie (2014-10-03)
K Maráková, J Piestanský, E Havránek, P Mikus
ABSTRACT

The advanced hyphenated method based on capillary electrophoresis (CE) on-line combined with electrospray ionization (ESI) and tandem mass spectrometry (MS/MS, here triple quadrupole, QqQ) was developed and applied in pharmaceutical analysis in this work. Under the optimized CE separation (background electrolyte: 50 mmol/L formic acid with pH 2.05), ESI ionization (sheath liquid: 0.1% v/v formic acid in 50% v/v aq methanol) and QqQ detection (100-160V fragmentor voltage, 15-25eV collision energy, depending on the type of analyte) conditions, highly efficient, reproducible, accurate, sensitive (sub microg/mL LODs) and selective (each analyte was unequivocally specified by two characteristic MS signals, i.e. qualifier, quantifier) determination of vitamins B was achieved. All vitamins B, namely thiamine, riboflavin, nicotinamide, nicotinic acid, pantothenic acid, pyridoxine, biotin, folic acid and cyanocobalamine, were simultaneously determined in various dosage forms (injection solution, tablets, and effervescent tablets) within ca. 16 min. The main benefits of the proposed CE-ESI-QqQ method in comparison with the CE-UV ones are considerably enhanced sensitivity and selectivity. Other benefits are low cost, simplicity, flexibility and environmental aspects when comparing CE-ESI-QqQ with HPLC-MS. Successful validation and application of the proposed CE-ESI-QqQ method suggest its routine use in highly effective and reliable multi-drug quality control.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Nicotinamide, ≥99.5% (HPLC)
Sigma-Aldrich
Nicotinamide, ≥98.5% (HPLC)
Sigma-Aldrich
Cetirizin dihydrochloride, ≥98.0% (HPLC)
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
Sigma-Aldrich
Folic acid, ≥97%
Sigma-Aldrich
Nicotinamide, BioReagent, suitable for cell culture, suitable for insect cell culture
Sigma-Aldrich
Folic acid, meets USP testing specifications
Sigma-Aldrich
Niacinamide, meets USP testing specifications
Sigma-Aldrich
Nicotinamide, ≥98% (HPLC), powder
Sigma-Aldrich
Folic acid, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture, ≥97%
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Supelco
Riboflavin (B2), analytical standard
Riboflavin for peak identification, European Pharmacopoeia (EP) Reference Standard
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
Niacinamide, Pharmaceutical Secondary Standard; Certified Reference Material
Nicotinamide, European Pharmacopoeia (EP) Reference Standard
Millipore
Bifido Selective Supplement B, suitable for microbiology
Supelco
Folic acid, Pharmaceutical Secondary Standard; Certified Reference Material
Folic acid, European Pharmacopoeia (EP) Reference Standard
USP
Folic acid, United States Pharmacopeia (USP) Reference Standard
USP
Niacinamide, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Nicotinic acid, meets USP testing specifications
Sigma-Aldrich
(−)-Riboflavin, meets USP testing specifications
Sigma-Aldrich
Nicotinic acid, ≥98%
Sigma-Aldrich
(−)-Riboflavin, from Eremothecium ashbyii, ≥98%