Skip to Content
Merck
  • 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
Hydroxyzine dihydrochloride, ≥97%
Sigma-Aldrich
Phosphoric acid, BioReagent, suitable for insect cell culture, 85%
Sigma-Aldrich
Phosphoric acid, BioUltra, ≥85% (T)
Sigma-Aldrich
Phosphoric acid, crystalline, ≥99.999% trace metals basis
Sigma-Aldrich
Phosphoric acid, ≥85 wt. % in H2O, ≥99.999% trace metals basis
Sigma-Aldrich
Phosphoric acid, 85 wt. % in H2O, 99.99% trace metals basis
Sigma-Aldrich
Sodium phosphate, 96%
Sigma-Aldrich
Terfenadine
Sigma-Aldrich
N6-Cyclopentyladenosine, solid
Sigma-Aldrich
Diphenhydramine hydrochloride, ≥98% (HPLC)
Sigma-Aldrich
Phosphoric acid-16O4 solution, 70 wt. % in D2O, 99.9 atom % 16O
Sigma-Aldrich
Fexofenadine hydrochloride, >98% (HPLC)
Sigma-Aldrich
Clemastine fumarate salt, ≥98% (HPLC)
Diphenhydramine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Supelco
Diphenhydramine hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Diphenhydramine hydrochloride, United States Pharmacopeia (USP) Reference Standard
USP
Fexofenadine hydrochloride, United States Pharmacopeia (USP) Reference Standard
Terfenadine, European Pharmacopoeia (EP) Reference Standard
USP
Olopatadine hydrochloride, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Phosphoric acid, ACS reagent, ≥85 wt. % in H2O
Sigma-Aldrich
Phosphoric acid, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥85%
Sigma-Aldrich
Olopatadine hydrochloride, ≥98% (HPLC)
Clemastine for system suitability, European Pharmacopoeia (EP) Reference Standard
Fexofenadine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Phosphoric acid, ACS reagent, ≥85 wt. % in H2O
Sigma-Aldrich
Ketotifen fumarate salt
Sigma-Aldrich
Triprolidine hydrochloride, ≥99%
Sigma-Aldrich
o-Phenylenediamine, Peroxidase substrate, ≥98.0%, powder
Sigma-Aldrich
o-Phenylenediamine, tablet, 20 mg substrate per tablet
Sigma-Aldrich
Promethazine hydrochloride