The fixed-dose combination artesunate (AS)–amodiaquine (AQ) is one of the most widely used treatments for uncomplicated falciparum malaria. It is currently proposed to the inclusion in the model list of essential medicines of World Health Organization and has been recently prequalified. Until now, no satisfactory method for the simultaneous determination of the two active ingredients had been available. Thus, a reversed phase high performance liquid chromatography for the quantitative determination of AQ and AS was developed and validated. Chromatography was performed using an end-capped octadecylsilyl silica gel column (100 × 4.6 mm, 3 μm) with a binary gradient using aqueous phase containing potassium dihydrogen phosphate (10 mM) and acetonitrile. Taking into consideration the physico-chemical characteristics of the two compounds related to their ionization, the use of a counter ion was necessary to ensure the retention of AQ in a reversed phase system simultaneously to AS. Thus, aqueous mobile phase was adjusted to pH 3.0 and the chosen counter ion was sodium 1-octanesulfonate (100 mM). In these conditions, the retention times were about 4 min for AQ and 10 min for AS with UV detection at 300 and 210 nm, respectively. Method was then validated according to ICH guideline (specificity/linearity/accuracy/precision) and potential interferences with excipients and degradation products were checked. It has also been used for an interlaboratory study involving seven African National Quality Control Laboratories and Afssaps (Agence française de sécurité sanitaire des produits de santé) laboratory. The results demonstrate that this rapid and simple method can be easily used by official laboratories for routine control, market survey and for the detection of potential substandard medicines which are very frequent in African countries.
The presence on the market of illegal products for slimming purposes or the treatment of overweight is a public health issue. These products may contain illicit chemicals in order to improve their effectiveness. Some of these weight-loss compounds are responsible for adverse events, including fatal outcomes. A general strategy for the analysis of any suspect formulation begins with a large screening for the general search of a wide range of compounds. A methodology for the qualitative and quantitative determination of 34 compounds in slimming preparations (such as dietary supplements or medicinal products) was used for the control of slimming formulations from the market, including over the Internet. The fast liquid chromatography system (ultra-high-pressure liquid chromatography) used a gradient of solvent (phosphate buffer and acetonitrile), a C18 endcapped column and a diode array detector. This system allows dual identification based on retention time and UV spectra. The analytical method is simple, fast and selective since 34 weight-loss compounds can be detected in a 15-min run time. Thus, 32 commercial slimming formulations were analysed using this method, allowing the detection and quantification of hazardous active substances: caffeine, clenbuterol, nicotinamide, phenolphthalein, rimonabant, sibutramine, didesmethylsibutramine, synephrine and yohimbine.