外文资料Standardless 1H NMR determination of pharmacologically active substances in dietary supplements and.pdfVIP
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Research article
Drug Testing
and Analysis
Received: 11 January 2012 Revised: 30 March 2012 Accepted: 30 March 2012 Published online in Wiley Online Library: 1 May 2012
() DOI 10.1002/dta.1367
4
0
0Standardless 1H NMR determination of
pharmacologically active substances in dietary
supplements and medicines that have been
illegally traded over the Internet
Yulia B Monakhova,a,b,c Thomas Kuballa,a Sigrid L?bell-Behrends,a
Sibylle Maixner,a Matthias Kohl-Himmelseher,a Winfried Rugea
and Dirk W Lachenmeiera*Dietary supplements and medicines are widely marketed over the Internet. Such products may be counterfeited and lack some
or all of the labelled ingredients, or, in the case of lifestyle supplements, illegally contain pharmacologically active substances,
such as anorectic or androgenic compounds. The market control – especially in the case of customs seizures – is complex, as
reference substances necessary for identification and calibration in traditional high performance liquid chromatography
(HPLC) or gas chromatography–mass spectrometry (GC-MS) analysis are often unavailable, or extremely expensive. In this
study, we introduce a 400 MHz 1H NMR methodology, which allows identification and quantitative estimation even without
such pure compound standards. The identification can be based on literature spectra, or if these data are unavailable, by
applying computational NMR spectra prediction. For standardless NMR determination, simple peak-area comparison of the
target compound with the TSP reference was used. The applicability was demonstrated for a wide range of compounds, such
as mesterolone, oxymetholone, sibutramine, monacolin K, vinpocetine, evodiamine, caffeine, kavain, and dehydroepiandros-
terone. The average relative standard deviations were 5.0% for peak area comparison, and 3.3% for external calibration with
standard substance. The method uncertainty is therefore higher in standardless determination, but acceptable for the
purpose of proving the presence
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