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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
o-Phenylenediamine, sublimed, ≥99%
Clemastine fumarate, European Pharmacopoeia (EP) Reference Standard
Promethazine for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Promethazine hydrochloride, vial of 25 mg, certified reference material, Cerilliant®
Epinastine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Promethazine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Desloratadine, powder, ≥98% (HPLC)
Sigma-Aldrich
Cyproheptadine hydrochloride sesquihydrate, 99%
Sigma-Aldrich
o-Phenylenediamine, flaked, 99.5%
Sigma-Aldrich
o-Phenylenediamine, tablet, 20 mg substrate per tablet
Sigma-Aldrich
Triprolidine hydrochloride, ≥99%
Sigma-Aldrich
o-Phenylenediamine, Peroxidase substrate, ≥98.0%, powder
Hydroxyzine hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Promethazine hydrochloride, United States Pharmacopeia (USP) Reference Standard
USP
Loratadine Related Compound A, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Epinastine hydrochloride, ≥98% (HPLC), solid
Sigma-Aldrich
Cyproheptadine hydrochloride sesquihydrate, ≥98% (TLC), solid
Sigma-Aldrich
Phosphoric acid solution, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
Promethazine hydrochloride
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
N,N′-Bis(3-methylphenyl)-N,N′-diphenylbenzidine, 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
Ketotifen fumarate salt
USP
Triprolidine hydrochloride, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Sodium phosphate ChemBeads
Supelco
Promethazine Hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Ketotifen for peak identification, European Pharmacopoeia (EP) Reference Standard
Ketotifen hydrogen fumarate, European Pharmacopoeia (EP) Reference Standard
Desloratadine, European Pharmacopoeia (EP) Reference Standard