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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
Acetic acid, 99.5-100.0%
Sigma-Aldrich
Methanol, SAJ first grade, ≥99.5%
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
Sigma-Aldrich
Methanol, JIS 300, ≥99.8%, for residue analysis
Sigma-Aldrich
Acetic acid, JIS special grade, ≥99.7%
Sigma-Aldrich
Acetic acid solution, 1 M, 1 N
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Nicotinic acid, SAJ special grade, ≥99.5%
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Methanol, SAJ special grade
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Ammonium acetate solution, 50 % (w/v), for copper determination
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Methanol, NMR reference standard
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Ammonia-14N, 99.99 atom % 14N
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Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Riboflavin, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Cetirizine dihydrochloride, ≥98% (HPLC)
Cetirizine for peak identification, European Pharmacopoeia (EP) Reference Standard
Pyridoxine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Riboflavin, European Pharmacopoeia (EP) Reference Standard
USP
Thiamine hydrochloride, United States Pharmacopeia (USP) Reference Standard
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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
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Acetic acid, ≥99.5%, FCC, FG
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Methanol, suitable for HPLC, gradient grade, 99.93%
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Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Nicotinic acid, ≥99.5% (HPLC)
Supelco
Methanol, analytical standard
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Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
Sigma-Aldrich
Ammonium acetate, 99.999% trace metals basis
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis