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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, glacial, puriss., 99-100%
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
Sigma-Aldrich
Ammonia solution, 7 N in methanol
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
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Methanol, ACS reagent, ≥99.8%
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Ammonia solution, 2.0 M in isopropanol
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Acetic acid, glacial, ≥99.99% trace metals basis
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Methanol, HPLC Plus, ≥99.9%
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Methanol, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
USP
Riboflavin, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Cetirizine dihydrochloride, ≥98% (HPLC)
Riboflavin, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Supelco
Pyridoxine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
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Riboflavin, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
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Cetirizine for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Nicotinic acid, European Pharmacopoeia (EP) Reference Standard
Supelco
Pyridoxine Hydrochloride (B6), analytical standard
Supelco
Nicotinic acid, analytical standard
Supelco
Thiamine Hydrochloride (B1), analytical standard
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Calcium-d-pantothenate, Pharmaceutical Secondary Standard; Certified Reference Material