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Pre-Column Derivatization HPLC Procedure for the Quantitation of Aluminium Chlorohydrate in Antiperspirant Creams Using Quercetin as Chromogenic Reagent.

Chromatographia (2014-10-04)
Eleni Kalogria, Athanasia Varvaresou, Spyridon Papageorgiou, Evaggelia Protopapa, Ioannis Tsaknis, Alexios Matikas, Irene Panderi
ABSTRACT

This article describes the development and validation of a selective high-performance liquid chromatography method that allows, after liquid-liquid extraction and pre-column derivatization reaction with quercetin, the quantification of aluminium chlorohydrate in antiperspirant creams. Chromatographic separation was achieved on an XTerra MS C18 analytical column (150 × 3.0 mm i.d., particle size 5 μm) using a mobile phase of acetonitrile:water (15:85, v/v) containing 0.08 % trifluoroacetic acid at a flow rate of 0.30 mL min-1. Ultraviolet spectrophotometric detection at 415 nm was used. The assay was linear over a concentration range of 3.7-30.6 μg mL-1 for aluminium with a limit of quantitation of 3.74 μg mL-1. Quality control samples (4.4, 17.1 and 30.6 μg mL-1) in five replicates from five different runs of analysis demonstrated intra-assay precision (% coefficient of variation <3.8 %), inter-assay precision (% coefficient of variation <5.4 %) and an overall accuracy (% recovery) between 96 and 101 %. The method was used to quantify aluminium in antiperspirant creams containing 11.0, 13.0 and 16.0 % (w/w) aluminium chlorohydrate, respectively.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Trifluoroacetic acid, suitable for HPLC, ≥99.0%
Sigma-Aldrich
Trifluoroacetic acid, ReagentPlus®, 99%
Supelco
Ammonium acetate, suitable for mass spectrometry (MS), LiChropur, eluent additive for LC-MS
Sigma-Aldrich
Quercetin, ≥95% (HPLC), solid
Sigma-Aldrich
Ammonium acetate, for molecular biology, ≥98%
Sigma-Aldrich
Trifluoroacetic acid, puriss. p.a., suitable for HPLC, ≥99.0% (GC)
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
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Ammonium acetate, ACS reagent, ≥97%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Supelco
Quercetin, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
Sigma-Aldrich
Trifluoroacetic acid, ≥99%, for protein sequencing
Sigma-Aldrich
Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
Sigma-Aldrich
Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
Sigma-Aldrich
Ammonium acetate, BioXtra, ≥98%
Sigma-Aldrich
Ammonium acetate, 99.999% trace metals basis
USP
Quercetin, United States Pharmacopeia (USP) Reference Standard
Supelco
Trifluoroacetic acid, analytical standard