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      Development and Validation of HPLC Method for the Simultaneous Determination of Five Food Additives and Caffeine in Soft Drinks

      International Journal of Analytical Chemistry
      Hindawi Publishing Corporation

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          Abstract

          Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC) conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0–7.0), flow rate (1.0–1.4 mL/min), and mobile phase ratio (85–95% acetate buffer). Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS-) 3V reverse phase column (250 × 4.6 mm, 5 μm) dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r 2 > 0.9962), accuracy (recoveries ≥ 95.75%), precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%), limits of detection (LODs), and limits of quantification (LOQs) parameters. LODs and LOQs for analytes were in the range of 0.10–0.19 μg/mL and 0.33–0.63 μg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.

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          Most cited references27

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          Statistical designs and response surface techniques for the optimization of chromatographic systems.

          This paper describes fundamentals and applications of multivariate statistical techniques for the optimization of chromatographic systems. The surface response methodologies: central composite design, Doehlert matrix and Box-Behnken design are discussed and applications of these techniques for optimization of sample preparation steps (extractions) and determination of experimental conditions for chromatographic separations are presented. The use of mixture design for optimization of mobile phases is also related. An optimization example involving a real separation process is exhaustively described. A discussion about model validation is presented. Some applications of other multivariate techniques for optimization of chromatographic methods are also summarized.
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            Experimental design in chromatography: a tutorial review.

            D. Hibbert (2012)
            The ability of a chromatographic method to successful separate, identify and quantitate species is determined by many factors, many of which are in the control of the experimenter. When attempting to discover the important factors and then optimise a response by tuning these factors, experimental design (design of experiments, DoE) gives a powerful suite of statistical methodology. Advantages include modelling by empirical functions, not requiring detailed knowledge of the underlying physico-chemical properties of the system, a defined number of experiments to be performed, and available software to accomplish the task. Two uses of DoE in chromatography are for showing lack of significant effects in robustness studies for method validation, and for identifying significant factors and then optimising a response with respect to them in method development. Plackett-Burman designs are widely used in validation studies, and fractional factorial designs and their extensions such as central composite designs are the most popular optimisers. Box-Behnken and Doehlert designs are becoming more used as efficient alternatives. If it is not possible to practically realise values of the factors required by experimental designs, or if there is a constraint on the total number of experiments that can be done, then D-optimal designs can be very powerful. Examples of the use of DoE in chromatography are reviewed. Recommendations are given on how to report DoE studies in the literature.
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              Simultaneous determination of water-soluble and fat-soluble synthetic colorants in foodstuff by high-performance liquid chromatography-diode array detection-electrospray mass spectrometry.

              An accurate method was developed for the simultaneous determination of water-Tartrazine, Amaranth, Ponceau 4R, Sunset Yellow FCF, and fat-Sudan (I-IV), synthetic soluble colorants in foodstuff. This method uses dimethylsulfoxide (DMSO) as the extraction solvent in the sample preparation process and high performance liquid chromatography (HPLC)-diode array detector (DAD)-electrospray mass spectrometry (ESI-MS), applying selected ion recording in positive/negative alternate mode to acquire mass spectral data, as the analytical technique. Linearity of around three orders in the magnitude of concentration was generally obtained. Detection and quantification limits of the investigated dyes, which were evaluated at signal to noise ratio of 3 for detection limit and 10 for quantification limit, were in the ranges of 0.01-4 and 0.03-11.2 ng, respectively. The recoveries of the eight synthetic colorants in four matrices ranged from 93.2 to 108.3%. Relative standard deviations of less than 8.2% were also achieved. This method has been applied successfully in the determination of water-soluble colorants in the soft drink and the delicious ginger, and fat-soluble dyes in chilli powders and chilli spices.
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                Author and article information

                Journal
                26989415
                4773534
                10.1155/2016/2879406
                This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

                Analytical chemistry
                Analytical chemistry

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