Wasik Andrzej, McCourt Josephine, Buchgraber Manuela
European Commission, DG Joint Research Centre, Institute for Reference Materials and Measurements, Retieseweg 111, 2440 Geel, Belgium.
J Chromatogr A. 2007 Jul 20;1157(1-2):187-96. doi: 10.1016/j.chroma.2007.04.068. Epub 2007 May 6.
A high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD) has been developed for the simultaneous determination of multiple sweeteners, i.e., acesulfame-K, alitame, aspartame, cyclamic acid, dulcin, neotame, neohesperidine dihydrochalcone, saccharin and sucralose in carbonated and non-carbonated soft drinks, canned or bottled fruits and yoghurt. The procedure involves an extraction of the nine sweeteners with a buffer solution, sample clean-up using solid-phase extraction cartridges followed by an HPLC-ELSD analysis. The trueness of the method was satisfactory with recoveries ranging from 93 to 109% for concentration levels around the maximum usable dosages for authorised sweeteners and from 100 to 112% for unauthorised compounds at concentration levels close to the limit of quantification (LOQs). Precision measures showed mean repeatability values of <4% (expressed as relative standard deviation) for highly concentrated samples and <5% at concentration levels close to the LOQs. Intermediate precision was in most cases <8%. The limits of detection (LODs) were below 15 microg g(-1) and the LOQs below 30 microg g(-1) in all three matrices. Only dulcin showed slightly higher values, i.e., LODs around 30 microg g(-1) and LOQs around 50 microg g(-1)
已开发出一种带蒸发光散射检测的高效液相色谱法（HPLC - ELSD），用于同时测定碳酸饮料和非碳酸饮料、罐装或瓶装水果及酸奶中的多种甜味剂，即乙酰磺胺酸钾、阿力甜、阿斯巴甜、环己基氨基磺酸、甘素、纽甜、新橙皮苷二氢查耳酮、糖精和三氯蔗糖。该方法包括用缓冲溶液萃取这九种甜味剂，使用固相萃取柱净化样品，然后进行HPLC - ELSD分析。对于授权甜味剂最大可用剂量附近的浓度水平，该方法的准确性令人满意，回收率在93%至109%之间；对于浓度接近定量限（LOQ）的未经授权化合物，回收率在100%至112%之间。精密度测定表明，高浓度样品的平均重复性值<4%（以相对标准偏差表示），浓度接近定量限时<5%。在大多数情况下，中间精密度<8%。在所有三种基质中，检测限（LOD）均低于15 μg g⁻¹，定量限低于30 μg g⁻¹。只有甘素的值略高，即检测限约为30 μg g⁻¹，定量限约为50 μg g⁻¹
