A Rapid Dialysis Method for Analysis of Artificial Sweeteners in Foods (2nd Report).

Following the previous report, a rapid dialysis method was developed for the extraction and purification of four artificial sweeteners, namely, sodium saccharide (Sa), acesulfame potassium (AK), aspartame (APM), and dulcin (Du), which are present in various foods. The method was evaluated by the addition of 0.02 g/kg of these sweeteners to a cookie sample, in the same manner as in the previous report. Revisions from the previous method were: reduction of the total dialysis volume from 200 to 100 mL, change of tube length from 55 to 50 cm, change of dialysate from 0.01 mol/L hydrochloric aqueous solution containing 10% sodium chloride to 30% methanol solution, and change of dialysis conditions from ambient temperature with occasional shaking to 50℃ with shaking at 160 rpm. As a result of these revisions, the recovery reached 99.3-103.8% with one hour dialysis. The obtained recovery yields were comparable to the recovery yields in the previous method with four hour dialysis.

[A rapid dialysis method for analysis of artificial sweeteners in food].

A simple and rapid dialysis method was developed for the extraction and purification of four artificial sweeteners, namely, sodium saccharin (Sa), acesulfame potassium (AK), aspartame (APM), and dulcin (Du), which are present in various foods. Conventional dialysis uses a membrane dialysis tube approximately 15 cm in length and is carried out over many hours owing to the small membrane area and owing to inefficient mixing. In particular, processed cereal products such as cookies required treatment for 48 hours to obtain satisfactory recovery of the compounds. By increasing the tube length to 55 cm and introducing efficient mixing by inversion at half-hour intervals, the dialysis times of the four artificial sweeteners, spiked at 0.1 g/kg in the cookie, were shortened to 4 hours. Recovery yields of 88.9-103.2% were obtained by using the improved method, whereas recovery yields were low (65.5-82.0%) by the conventional method. Recovery yields (%) of Sa, AK, APM, and Du, spiked at 0.1 g/kg in various foods, were 91.6-100.1, 93.9-100.1, 86.7-100.0 and 88.7-104.7 using the improved method.

Imitation of biomembranes on the basis of cholic acid and endogenic thermostable protein complex in biopartitioning micellar chromatography.

The structure of biomembranes was imitated by introducing nonionic surfactant polyoxyethylene (23) dodecylether, cholic acid and endogenic thermostable protein complex (14-65 kDa) into the mobile phase. The influence of concentration of these additives on the retention of the model compounds was studied. The competing interaction of cholic acid and endogenic thermostable protein complex in the lipid bilayer model was revealed on the basis of chromatographic data. The values of efficiency of the chromatographic column regarding solutes were increased by addition of endogenic thermostable protein complex to the mobile phase containing Brij-35 and cholic acid.

Enhancement of saccharin removal from aqueous solution by activated carbon adsorption with ultrasonic treatment.

This study investigates the use of ultrasonication as a pretreatment process and its effect on the adsorption characteristics of saccharin onto activated carbon (AC). Ultrasonic decomposition of saccharin was performed at a frequency of 500 kHz under argon and O2/N2 (20/80 vol%) atmospheres. Adsorption was carried out using a commercial activated carbon. The behavior of total organic carbon (TOC) during ultrasonication was investigated. Saccharin removal after 180 min of ultrasonication under Ar and O2/N2 atmospheres are 38% and 26%, respectively, while the amount of saccharin removed by activated carbon adsorption without US pretreatment is 40% after 16 h. After 16 h of AC adsorption with 180 min of ultrasonic pretreatment under Ar and O2/N2 atmospheres, both removal ratios increased to 75%. These results indicated that the pretreatment of sonication under O2/N2 leads to the increase in the amount of saccharin adsorbed on AC. On the other hand, the TOC removal by decomposition by ultrasound is not more than 5% in both Ar and O2/N2 atmospheres after 180 min ultrasonication. However, the TOC removal increased to 54% and 69% after 16 h of adsorption of saccharin pretreated by ultrasonication for 180 min under Ar and O2/N2 atmospheres, respectively. About 13% and 16% TOC removal in Ar and in O2/N2, respectively, were achieved due to adsorption of the by-products. It is considered that the improvement in TOC removal is also brought about by the formation of the by-products that were adsorbed onto AC.

Separation and simultaneous determination of four artificial sweeteners in food and beverages by ion chromatography.

In this paper, the separation and determination of four artificial sweeteners (aspartame, sodium cyclamate, acesulfame-K and sodium saccharin) by ion chromatography coupled with suppressed conductivity detector is reported. The four artificial sweeteners were separated using KOH eluent generator. Due to the use of eluent generator, very low conductance background conductivity can be obtained and sensitivity of sweeteners has been greatly improved. Under the experimental condition, several inorganic anions, such as F-, Cl-, NO3-, NO2-, Br-, SO4(2)-, PO4(3)- and some organic acid such as formate, acetate, benzoate, and citrate did not interfere with the determination. With this method, good linear relationship, sensitivity and reproducibility were obtained. Detection limits of aspartame, sodium cyclamate, acesulfame-K, sodium saccharin were 0.87, 0.032, 0.019, 0.045 mg/L, respectively. Rate of recovery were between 98.23 and 105.42%, 99.48 and 103.57%, 97.96 and 103.23%, 98.46 and 102.40%, respectively. The method has successfully applied to the determination of the four sweeteners in drinks and preserved fruits.

Reversed-phase high-performance liquid chromatographic separation of saccharin, caffeine and benzoic acid using non-linear programming.

A method is described which allows a chromatographic assay to be optimized with respect to the time needed to complete an analysis, while maintaining good resolution. The method introduces an operational research technique called linear programming. It was used to optimize the eluent composition for the assay of saccharin, caffeine and benzoic acid and resulted in a significant reduction in the analysis time.

The mutagenicity of saccharin impurities. I. Detection of mutagenic activity.

Sodium saccharin, ortho-toluenesulfonamide and impurities extracted from commercially produced saccharin with water and organic solvents were tested for mutagenicity with strains of Salmonella typhimurium. The organic solvent soluble impurities exhibited strong mutagenic activity for TA98 and slight activity for TA100. Mutagenic activity for S. typhimurium TA98 was demonstrated in extracts of some but not all lots of sodium saccharin produced by both Maumee and Remsen-Fahlberg processes. The significance of the mutagenic impurity to the carcinogenicity of saccharin is discussed.