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Merck
  • 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
초록

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
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제품 설명

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Acetic acid-12C2, 99.9 atom % 12C
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Cetirizine dihydrochloride, ≥98% (HPLC)
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Riboflavin, Pharmaceutical Secondary Standard; Certified Reference Material
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Thiamine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
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Pyridoxine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
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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
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Cetirizine for peak identification, European Pharmacopoeia (EP) Reference Standard
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Thiamine hydrochloride, United States Pharmacopeia (USP) Reference Standard
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Nicotinic acid, ≥99.5% (HPLC)
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Acetic acid, analytical standard
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Methanol, analytical standard
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Thiamine hydrochloride, tested according to Ph. Eur.
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Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
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Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
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Ammonium formate, ≥99.995% trace metals basis
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Thiamine hydrochloride, ≥98%, FCC, FG
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Acetic acid, natural, ≥99.5%, FG
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Acetic acid, ≥99.5%, FCC, FG
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Ammonium acetate, 99.999% trace metals basis
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Ammonium acetate, LiChropur, eluent additive for LC-MS
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Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
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Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
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Nicotinic acid, analytical standard
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Thiamine Hydrochloride (B1), analytical standard
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Pyridoxine Hydrochloride (B6), analytical standard
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Methanol, anhydrous, 99.8%