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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

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