DEVELOPMENT AND VALIDATION OF AN HPLC METHOD FOR THE DETERMINATION OF ACESULFAME K AND SACCHARIN IN CONFECTIONERY WITH NO ADDED SUGAR
VIOLETA NOUR 1*, ION TRANDAFIR 2, MIRA ELENA IONICA 1 (1)UNIVERSITY OF CRAIOVA, FACULTY OF HORTICULTURE, STR. A.I.CUZA NR.13, CRAIOVA, ROMANIA (2)UNIVERSITY OF CRAIOVA, FACULTY OF CHEMISTRY, BD.CALEA BUCURESTI, NO.107I, CRAIOVA, ROMANIA *CORRESPONDING AUTHOR: VIONOUR@CENTRAL.UCV.RO
A simple, selective, and precise reverse phase high performance liquid chromatographic method has been developed for the simultaneous determination of acesulfame K and saccharin in the confectionery with no added sugar (Solano candies). For analysis, the sample is extracted or diluted with water, and the solution of the sample with the two sweeteners is purified by an extraction with Carrez reagents. The chromatographic separation was achieved with potassium dihydrogen orthophosphate buffer (pH = 4.3) and acetonitrile (98:2, v/v) as mobile phase, a DS HYPERSIL C18 5 ?m column (250 mm ? 4.6 mm) and diode array detection at 220 nm. The analysis time was less than 20 min. The calibration curves showed good linearity over the concentration range of 0-40 mg/L. The correlation coefficients were > 0.999914 in each case. The method was validated with respect to sensitivity, linearity range, reproducibility, repeatability, recovery and robustness. There have been obtained average recovery values of 93.0325% for acesulfame K and 93.7067% for saccharin for an addition level of 5 mg/L in the sample solution (the final concentration in sample 227 mg/kg acesulfame K and 234 mg/kg saccharin). The method proved high fidelity and stability, and the detection limit was 1 mg/kg for acesulfame K and 0.4 mg/kg for saccharin for a signal to noise ratio of 3.
