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Validation of a quantitative NMR method for suspected counterfeit products exemplified on determination of benzethonium chloride in grapefruit seed extracts
Uppsala University, Disciplinary Domain of Medicine and Pharmacy, Faculty of Pharmacy, Department of Medicinal Chemistry, Analytical Pharmaceutical Chemistry.
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2008 (English)In: Journal of Pharmaceutical and Biomedical Analysis, ISSN 0731-7085, Vol. 47, no 4-5, 958-961 p.Article in journal (Refereed) Published
Abstract [en]

A H-1-nuclear magnetic resonance (NMR) spectroscopy method for quantitative determination of benzethonium chloride (BTC) as a constituent of grapefruit seed extract was developed. The method was validated, assessing its specificity, linearity, range, and precision, as well as accuracy, limit of quantification and robustness. The method includes quantification using an internal reference standard, 1,3,5-trimethoxybenzene, and regarded as simple, rapid, and easy to implement. A commercial grapefruit seed extract was studied and the experiments were performed on spectrometers operating at two different fields, 300 and 600 MHz for proton frequencies, the former with a broad band (BB) probe and the latter equipped with both a BB probe and a CryoProbe (TM). The concentration average for the product sample was 78.0, 77.8 and 78.4 mg/ml using the 300 BB probe, the 600 MHz BB probe and CryoProbe (TM), respectively. The standard deviation and relative standard deviation (R.S.D., in parenthesis) for the average concentrations was 0.2 (0.3%), 0.3 (0.4%) and 0.3 mg/ml (0.4%), respectively.

Place, publisher, year, edition, pages
2008. Vol. 47, no 4-5, 958-961 p.
Keyword [en]
quantification, NMR, validation, benzethonium chloride, grapefruit seed extract, internal reference standard
National Category
Pharmaceutical Sciences
URN: urn:nbn:se:uu:diva-17638DOI: 10.1016/j.jpba.2008.03.021ISI: 000257220300049PubMedID: 18456447OAI: oai:DiVA.org:uu-17638DiVA: diva2:45409
Available from: 2008-07-30 Created: 2008-07-30Bibliographically approved

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Arvidsson, TorbjörnHakkarainen, Birgit
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