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  • Development and validation of an ultra-performance liquid chromatography method for simultaneous analysis of 20 antihistaminics in dietary supplements.

Development and validation of an ultra-performance liquid chromatography method for simultaneous analysis of 20 antihistaminics in dietary supplements.

Biomedical chromatography : BMC (2014-08-01)
Jung Yeon Kim, Jung-Ah Do, Ji Yeon Choi, Sooyeul Cho, Woo-Seong Kim, Chang-Yong Yoon
ABSTRACT

The purpose of this study was to develop and validate an ultra-performance liquid chromatography method for simultaneous analysis of 20 antihistamines (illegal additives) in dietary supplements. The limits of detection and quantitation of the method ranged from 1.5 to 2.5 µg/mL and from 20.0 to 50.0 µg/mL, respectively. The determination coefficient was >0.999, precisions were 0.2-5.1% (intra-day) and 0.1-8.8% (inter-day), and accuracies were 84.5-111.2% (intra-day) and 91.9-112.0% (inter-day). The mean recoveries of 20 targeted compounds from dietary supplements ranged from 75.4 to 119.3%. The relative standard deviations were <6.6% and complied with established international guidelines. The relative standard deviation of stability was <0.8%. Fifty-two commercially available dietary supplements were evaluated using this method, and were found to have none of the 20 antihistamines in significant abundance.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Sodium phosphate ChemBeads
Sigma-Aldrich
o-Phenylenediamine, sublimed, ≥99%
Sigma-Aldrich
Desloratadine, powder, ≥98% (HPLC)
Clemastine fumarate, European Pharmacopoeia (EP) Reference Standard
Promethazine for peak identification, European Pharmacopoeia (EP) Reference Standard
Epinastine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Phosphoric acid solution, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
o-Phenylenediamine, flaked, 99.5%
Sigma-Aldrich
N,N′-Bis(3-methylphenyl)-N,N′-diphenylbenzidine, 99%
Sigma-Aldrich
Cyproheptadine hydrochloride sesquihydrate, 99%
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube
Sigma-Aldrich
o-Phenylenediamine, Peroxidase substrate, ≥98.0%, powder
Sigma-Aldrich
o-Phenylenediamine, tablet, 20 mg substrate per tablet
Sigma-Aldrich
Ketotifen fumarate salt
Sigma-Aldrich
Triprolidine hydrochloride, ≥99%
Sigma-Aldrich
Promethazine hydrochloride
Sigma-Aldrich
Epinastine hydrochloride, ≥98% (HPLC), solid
Sigma-Aldrich
Cyproheptadine hydrochloride sesquihydrate, ≥98% (TLC), solid
Promethazine hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Loratadine Related Compound A, United States Pharmacopeia (USP) Reference Standard
Hydroxyzine hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Triprolidine hydrochloride, United States Pharmacopeia (USP) Reference Standard
Ketotifen hydrogen fumarate, European Pharmacopoeia (EP) Reference Standard
Ketotifen for peak identification, European Pharmacopoeia (EP) Reference Standard
Desloratadine, European Pharmacopoeia (EP) Reference Standard
Supelco
Promethazine Hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Promethazine hydrochloride, United States Pharmacopeia (USP) Reference Standard
Supelco
Diphenhydramine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Phosphoric acid-16O4 solution, 70 wt. % in D2O, 99.9 atom % 16O
Sigma-Aldrich
Olopatadine hydrochloride, ≥98% (HPLC)