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  • Development and application of a validated stability-indicating high-performance liquid chromatographic method using photodiode array detection for simultaneous determination of granisetron, methylparaben, propylparaben, sodium benzoate, and their main degradation products in oral pharmaceutical preparations.

Development and application of a validated stability-indicating high-performance liquid chromatographic method using photodiode array detection for simultaneous determination of granisetron, methylparaben, propylparaben, sodium benzoate, and their main degradation products in oral pharmaceutical preparations.

Journal of AOAC International (2011-12-15)
Ismail Hewala, Hamed El-Fatatry, Ehab Emam, Mokhtar Mabrouk
ABSTRACT

A simple, rapid, and sensitive RP-HPLC method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron), sodium benzoate, methylparaben, propylparaben, and 4-hydroxybenzoic acid (the main degradation product of parabens) in granisetron oral drops and solutions. The separation of the compounds was achieved within 8 min on a SymmetryShield RP18 column (100 x 4.6 mm id, 3.5 microm particle size) using the mobile phase acetonitrile--0.05 M KH2PO4 buffered to pH 3 using H3PO4 (3+7, v/v). The photodiode array detector was used to test the purity of the peaks, and the chromatograms were extracted at 240 nm. The method was validated, and validation acceptance criteria were met in all cases. The robust method was successfully applied to the determination of granisetron and preservatives, as well as their degradation products in different batches of granisetron oral drops and solutions. The method proved to be sensitive for determination down to 0.04% (w/w) of granisetron degradation product relative to granisetron and 0.03% (w/w) 4-hydroxybenzoic acid relative to total parabens.

MATERIALS
Product Number
Brand
Product Description

Supelco
Methyl Paraben, PESTANAL®, analytical standard
Supelco
Propylparaben, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Methylparaben, Pharmaceutical Secondary Standard; Certified Reference Material
Propyl parahydroxybenzoate, European Pharmacopoeia (EP) Reference Standard
Methyl parahydroxybenzoate, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Sodium benzoate, BioXtra, ≥99.5%
Sigma-Aldrich
Methyl 4-hydroxybenzoate, ≥99%, FCC
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Propyl 4-hydroxybenzoate, ≥99%
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Sodium benzoate, ReagentPlus®, 99%
Sigma-Aldrich
Sodium benzoate, purum p.a., ≥99.0% (NT)
Sigma-Aldrich
Methyl 4-hydroxybenzoate, tested according to Ph. Eur.
Sigma-Aldrich
Propyl 4-hydroxybenzoate, tested according to Ph. Eur.
Sigma-Aldrich
Methyl 4-hydroxybenzoate, analytical standard
Sigma-Aldrich
Methyl 4-hydroxybenzoate, ReagentPlus®, ≥99.0%, crystalline
Sigma-Aldrich
Methyl 4-hydroxybenzoate, BioReagent, suitable for insect cell culture
Sigma-Aldrich
Methyl 4-hydroxybenzoate, BioXtra, ≥99.0% (titration)
Sigma-Aldrich
Propyl 4-hydroxybenzoate, BioXtra
Supelco
Granisetron Hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Sodium benzoate, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Sodium benzoate, puriss., meets analytical specification of Ph. Eur., BP, FCC, E211, 99.0-100.5% (calc. to the dried substance), powder