Determination of free and total carbohydrate profile in soluble coffee.

A liquid chromatographic (LC) method was evaluated for the determination of free and total carbohydrates in soluble coffee. Samples are solubilized in water for free carbohydrates or hydrolyzed with 1.00N hydrochloric acid for total carbohydrates. An aliquot of the sample solution is analyzed on a pellicular anion-exchange polystyrene-divinylbenzene column using pure water as the mobile phase. Carbohydrates are quantitated by a pulsed amperometric detector. All major carbohydrates found in soluble coffee are determined in a single run. The technique allowed the detection of fraudulent addition of coffee husks or parchments as well as cereals or caramelized sugar for the 63 commercial products analyzed. High levels of free mannitol, free fructose, free glucose, sucrose, total glucose, and total xylose are a good indication of adulteration. Data were compared with those obtained from separate enzymatic determinations and from a different LC procedure. A close agreement among the methods was observed. However, the original method was superior in precision and was the only procedure that enabled the quantitation of all major carbohydrates. The technique is, therefore, a very powerful tool for routine analysis and for purity assessment of soluble coffee.

Adulteration of soluble coffee with coffee husks and parchments.

Commercial soluble coffee can be adulterated with coffee husks or parchments. Xylose is a good tracer for this type of mispractice. The analysis of total xylose in a wide selection of green beans and the assessment of its fate during processing allowed the derivation of a maximum total xylose limit of 0.40%, above which a soluble coffee should be considered as adulterated. Out of the 700 commercial soluble coffees analyzed, 81 exhibited a total xylose level above this limit. Of the samples with total xylose level lower than the limit, 99% displayed concentrations in free mannitol and total glucose below 0.30 and 2.10%, respectively.

Determination of aspartame and its major decomposition products in foods.

A liquid chromatographic procedure already evaluated in a preceding study for the analysis of acesulfam-K is also suitable for the determination of the intense sweetener aspartame in tabletop sweetener, candy, fruit beverage, fruit pulp, soft drink, yogurt, cream, cheese, and chocolate preparations. The method also allows the determination of aspartame's major decomposition products: diketopiperazine, aspartyl-phenylalanine, and phenylalanine. Samples are extracted or diluted with water and filtered. Complex matrixes are centrifuged or clarified with Carrez solutions. An aliquot of the extract is analyzed on a reversed-phase muBondapak C18 column using 0.0125M KH2PO4 (pH 3.5)-acetonitrile ([85 + 15] or [98 + 2]) as mobile phase. Detection is performed by UV absorbance at 214 nm. Recoveries ranged from 96.1 to 105.0%. Decomposition of the sweetener was observed in most food samples. However, the total aspartame values (measured aspartame + breakdown products) were within -10% and +5% of the declared levels. The repeatabilities and the repeatability coefficients of variation were, respectively, 1.00 mg/100 g and 1.34% for products containing less than 45 mg/100 g aspartame and 4.11 mg/100 g and 0.91% for other products. The technique is precise and sensitive. It enables the detection of many food additives or natural constituents, such as other intense sweeteners, organic acids, and alkaloids, in the same run without interfering with aspartame or its decomposition products. The method is consequently suitable for quality control or monitoring.

Determination of acesulfam-K in foods.

A liquid chromatographic method was evaluated for the determination of the intense sweetener acesulfam-K in tabletop sweetener, candy, soft drink, fruit juice, fruit nectar, yogurt, cream, custard, chocolate, and biscuit commercial preparations. Samples are extracted or simply diluted with water and filtered. Complex matrixes need a clarification step with Carrez solutions. An aliquot of the extract is analyzed on a reversed-phase mu Bondapak C18 column using 0.0125M KH2PO4 (pH 3.5)-acetonitrile (90 + 10) as mobile phase. Detection is performed by UV absorbance at 220 nm. Recoveries ranged from 95.2 to 106.8%. With one exception, all analyzed values were within +/- 15% of the declared levels. The repeatabilities and the repeatability coefficients of variation were, respectively, 0.37 mg/100 g and 0.98% for products containing less than 40 mg/100 g acesulfam-K and 2.43 mg/100 g and 1.29% for other products. The same procedure also allowed detection of many food additives or natural constituents, such as other intense sweeteners, organic acids, and alkaloids, in a single run without interfering with acesulfam-K. The method is simple, rapid, precise, and sensitive; therefore, it is suitable for routine analyses.