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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
Ammonium acetate, BioXtra, ≥98%
Sigma-Aldrich
Nicotinic acid, meets USP testing specifications
Sigma-Aldrich
Nicotinic acid, ≥98%
Sigma-Aldrich
(−)-Riboflavin, BioReagent, suitable for cell culture, suitable for insect cell culture, ≥98%
Sigma-Aldrich
(−)-Riboflavin, meets USP testing specifications
Sigma-Aldrich
(−)-Riboflavin, from Eremothecium ashbyii, ≥98%
Sigma-Aldrich
Ammonium acetate, for molecular biology, ≥98%
Sigma-Aldrich
Thiamine hydrochloride, reagent grade, ≥99% (HPLC)
Sigma-Aldrich
Thiamine hydrochloride, meets USP testing specifications
Sigma-Aldrich
Thiamine hydrochloride, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Sigma-Aldrich
Nicotinic acid, ≥99.5% (HPLC)
Supelco
Methanol, analytical standard
Sigma-Aldrich
Pyridoxine hydrochloride, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture
Sigma-Aldrich
Pyridoxine hydrochloride, ≥98% (HPLC)
Sigma-Aldrich
Pyridoxine hydrochloride, meets USP testing specifications
Supelco
Thiamine Hydrochloride (B1), analytical standard
Supelco
Pyridoxine Hydrochloride (B6), analytical standard
Sigma-Aldrich
Nicotinic acid, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture, ≥98%
Supelco
Nicotinic acid, analytical standard
Sigma-Aldrich
Nicotinic acid, SAJ special grade, ≥99.5%
Supelco
Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Pyridoxine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Riboflavin, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ammonium acetate solution, 50 % (w/v), for copper determination
Sigma-Aldrich
Ammonium formate, SAJ first grade, ≥95.0%
Riboflavin, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
USP
Thiamine hydrochloride, United States Pharmacopeia (USP) Reference Standard