Summary
Three HPLC methods were optimised for the determination of citric acid, succinic acid and ascorbic acid using a photodiode array detector and fructose, glucose and sucrose using a refractive index in twenty eight citrus juices. The analysis was completed in <16 min. Two different harvests were taken into account for this study. For the season 2011, ascorbic acid content was comprised between 19.4 and 59 mg vitamin C/100 mL; meanwhile for the season 2012, the content was slightly higher for most of the samples ranging from 33.5 to 85.3 mg vitamin C/100 mL. Moreover, the citric acid content in orange juices ranged between 9.7 and 15.1 g L−1, while for clementines the content was clearly lower (i.e. from 3.5 to 8.4 g L−1). However, clementines showed the highest sucrose content with values near to 6 g/100 mL. Finally, a cluster analysis was applied to establish a classification of the citrus species.
Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) has been employed to carry out the determination of both major anions and cations in water samples. The anions quantification has been performed by means of a new automatic accessory. In this device chloride has been determined by continuously adding a silver nitrate solution. As a result solid silver chloride particles are formed and retained on a Nylon filter inserted in the line. The emission intensity is read at a silver characteristic wavelength. By plotting the drop in silver signal versus the chloride concentration, a straight line is obtained. As regards bicarbonate, this anion has been on-line transformed into carbon dioxide with the help of a 2.0 mol L-1 nitric acid stream. Carbon signal is linearly related with bicarbonate concentration. Finally, information about sulfate concentration has been achieved by means of the measurement of sulfur emission intensity. All the steps have been simultaneously and automatically performed. With this setup detection limits have been 1.0, 0.4 and 0.09 mg L-1 for chloride, bicarbonate and sulfate, respectively. Furthermore, it affords good precision with RSD below 6 %. Cations (Ca, Mg, Na and K) concentration, in turn, has been obtained by simultaneously reading the emission intensity at characteristic wavelengths. The obtained limits of detection have been 8 x 10-3 , 2 x 10-3 , 8 x 10-4 and 10-2 mg L-1 for sodium, potassium, magnesium and calcium, respectively. As regards sample throughput about 30 samples h-1 can be analyzed. Validation results have revealed that the obtained concentrations for these anions are not significantly different as compared to the data provided by conventional methods. Finally, by considering the data for anions and cations precise ion balances have been obtained for well and mineral water samples.
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