Saccharin added

Nakamura (59) had developed a procedure for the isolation and determination of saccharin in foods by measuring fluorescence at UlO nm (excitation at 277 nm). However recovery of saccharin added to 23 types of food ranged from 82 to 98. ... 

Table II. Survey of Saccharin Added to Candied Fruits Bought in the Market...

Other electrolytes have been tested. Saccharin sodium hydrate was recently proposed by Bazzaoui et al. [91], as well as saccharin added to oxalic acid as supporting electrolyte [92]. In this latter case an improvement with respect to the oxalic acid electrolyte was attributed to a reinforcement of the barrier effect of the passive layer. Less usual ways have been explored with ionic liquids as media for electropolymerization. Formation of highly conducting PPy on iron in l-butyl-3-methylimidazolium hexafluorophosphate was reported [93] however, it does not seem promising because such solvents are expensive and also because adhesion to the metal is poor. 

There is no known method for accurately determining fruit juice content. For the determination of citrus juices in beverages it is shown by Stern that the percentage and alkalinity of the ash is of no value because of the influence of the alkalinity from sodium benzoate or sulphites added as preservatives and saccharin added in the presence of sodium bicarbonate. The phosphoric anhydride content is independent of these factors and the following table summarises the data for the range to be expected in natural juices. 

For example, if saccharin (33) is methylated in benzene suspension, then only iV-methylsaccharin is isolated. If an ethereal saccharin solution is added to a concentrated solution of diazomethane in excess, then 10% of 0-methylsaecharin (34) can be detected in addition to the A"-raethy] derivative. Finally, if the diazomethane solution is gradually added to a saturated ethereal solution of saccharin, the proportion of 0-methylation increases to 24%. " ... 

When diazomethane is slowly added to excess lactam, the anions formed can interact with unreacted lactam by means of hydrogen bonds to form ion pairs similar to those formed by acetic acid-tri-ethylamine mixtures in nonpolar solvents. The methyldiazonium ion is then involved in an ion association wdth the mono-anion of a dimeric lactam which is naturally less reactive than a free lactam anion. The velocity of the Sn2 reaction, Eq. (7), is thus decreased. However, the decomposition velocity of the methyldiazonium ion, Eq. (6a), is constant and, hence, the S l character of the reaction is increased which favors 0-methylation. It is possible that this effect is also involved in kinetic dependence investigations have shown that with higher saccharin concentrations more 0-methylsaccharin is formed. 

To a suspension of (45)-azetidin-2-one-4-carboxyIic acid (0.1 mol) and saccharin (1 g) in chloroform (200ml) was added HMDS (0.4mol), and the mixture was heated under reflux for 1.5 h. The excess HMDS was removed under reduced pressure, and the residue was distilled to afford the protected /1-lactam (0.089mol. 89%). b.p. 74-76 °C/0.08mmHg. 

Sweeteners such as sodium saccharin are added for taste. Other flavors are usually strong essential oils in the mint family. 

Chen et al. (1997a) analysed sodium saccharin in soft drinks, orange juice and lemon tea after filtration by injection into an ion-exclusion column with detection at 202 nm. Recoveries of 98-104% were obtained. They reported that common organic acids like citric and malic and other sweeteners did not interfere. Qu et al. (1999) determined aspartame in fruit juices, after degassing and dilution in water, by IC-PAD. The decomposition products of aspartame, aspartic acid and phenylanaline were separated and other sweeteners did not interfere. The recoveries of added aspartame were 77-94%. Chen et al. (1997b) separated and determined four artificial sweeteners and citric acid. 

While continuing to mix the solution, the para-ben/glycol solution, the remaining propylene glycol, artificial strawberry flavor, artificial banana flavor, saccharin sodium, citric acid anhydrous, and sodium citrate dihydrate are added and mixed until dissolved. 

Clarification of extracts can be accomplished with Carrez reagents (44). Purification has been performed by solid phase or partition. Wu et al. (47) absorbed saccharin onto ODS-4 cartridges and then eluted with methanol phosphate buffer. Puttemans et al. (28,50) extracted saccharin from soft drinks and yogurt by ion-pair extraction with tri-n-octylamine and back-extraction to an aqueous phase with perchlorate. Tereda and Sakabe (48) used cetrimide and Sep-Pak Cl8 in the cleanup of saccharin in coffee drink. The column was preconditioned with methanol, water, and 5 mM cetrimide. The sample, diluted in phosphate buffer pH 3.0 containing cetrimide was poured into the cartridge, washed with water, and eluted with acetonitrile water (1 1, v/v). Moriyasu et al. (40) added n-propylammonium bromide to the extract, passed it through a Bond Elut Cl 8 column, and eluted the sweetener with a mixture of methanol-water (4 6, v/v). The eluate was passed through a Bond Elut SAX column and washed with 0.5% phosphoric acid and water, and the sweetener was eluted with 0.3 N hydrochloric acid. 

Reverse-phase chromatography has been used extensively for the determination of saccharin. Smyly et al. (30) and Eng et al. (39) used /rBondapak Cl 8 and 5% acetic acid for the determination of saccharin. Based on this work, an Association of Official Analytical Chemists (AOAC) collaborative study was conducted, and the method using a mobile phase buffered to pH 3 with sodium acetate and modified with 3% isopropanol was adopted. Webb and Beckman (61) used this method successfully for the separation of saccharin from aspartame, caffeine, sodium benzoate, and artificial colors and flavors. Veerabhadrarao et al. (27) added methanol to the mobile phase (methanol acetic acid water, 4 1 1, v/v) for improved separation of saccharin from caffeine, benzoic and p-hydroxybenzoic acids, vanillin, aspartame, acesulfame-K, and dulcin. Saccharin was also determined using LiChrosorb Cl8 and 4 6 v/v methanol phosphate buffer,... 

Ion-pair chromatography has also been used for the determination of dulcin. Wu et al. (47) added the ion pair tetraethylammonium hydroxide to the mobile-phase methanol 85% phosphoric acid, pH 6 (2 8), for the separation of dulcin from saccharin, cyclamate, aspartame, and acesulfame-K on /xBondapak 08. Herrmann et al. (24) separated dulcin from saccharin, cyclamate, and aspartame on Hypersil MOS 3 using a mobile phase consisting of 5 mM tetrabutylam-... 

Soft drinks will contain sodium (from water and added sodium salts, e.g. benzoate, saccharin, citrate, CMC), calcium and magnesium (from water and fruit materials) and potassium and phosphate (from fruit materials). 

Addition of substances of the former class may be detected by the increased proportion of saccharine substances in the bread when the added sugar has not been entirely decomposed. 

Analysis of refined sugars is mostly reduced to the determination of the saccharose by direct polarisation. In some cases the ash and moisture are also determined, and in rare instances other determinations may be necessary, such as that of the reducing sugars (invert sugar and, perhaps, glucose or lactose added as adulterant) or raifinose a test for saccharin is occasionally required. 

The bulk of the filtrate is distilled off and the remaining liquid evaporated to dryness in a porcelain dish on a water-bath, together with a few c.c. of the distillate with which the distilling flask is rinsed The residue is dissolved in the hot in about 50 c.c. of distilled water and while the dish is kept on a water-bath and the liquid stirred with a rod, an approximately normal solution of permanganate is added drop by drop. The addition of permanganate, which is for the purpose of destroying any substances extracted along with the saccharin, is discontinued when the liquid remains pink for some minutes. 

Acesulfame K is, in contrast, sufficiently heat stable to be added at the beginning of the boil. Unfortunately, the sweetness profile is not as good. One approach to using intense sweeteners is to use a combination of ingredients, and common combinations such as aspartame and acesulfame K or aspartame and saccharin are used. Where they are legal, cyclamates are also used in this application. 

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