A new reversed-phase ultraperformance liquid chromatography method with a photodiode array detector was developed for the quantification of ascorbic acid (AA) and caffeine (CAF) in 11 different commercial drinks consisting of one energy drink and 10 ice tea drinks. Separation of the analyzed AA and CAF with an internal standard, caffeic acid, was performed on a Waters BEH C column (100 mm × 2.1 mm, 1.7 μm i.d.), using a mobile phase consisting of acetonitrile and 0.2M HPO (11:89, v/v) with a flow rate of 0.25 mL/min and an injection volume of 1.0 μL. Calibration graphs for AA and CAF were computed from the peak area ratio of AA/internal standard and CAF/internal standard detected at 244.0 nm and 273.6 nm, respectively. The developed reversed-phase ultraperformance liquid chromatography method was validated by analyzing standard addition samples. The proposed reversed-phase ultraperformance liquid chromatography method gave us successful results for the quantitative analysis of commercial drinks containing AA and CAF substances.
The need to enhance food safety has led to major advancements in pesticide productions, and though many benefits have been gained, environmental contamination has also risen from these chemicals that tend to persist in the environment. Some pesticides, together with other chemicals commonly called endocrine disruptor compounds, block the receptor sites of hormones or mimic displaced hormones, leading to imbalanced hormonal levels that result in health disorders and diseases. These chemicals occur at trace levels and are not directly detected by conventional analytical methods. A dispersive liquid-liquid microextraction method was therefore developed for preconcentration of 12 analytes including hormones, endocrine disruptor compounds, and pesticides, to be analyzed by gas chromatography mass spectrometry. This was achieved by optimizing parameters such as extractor solvent type and amount, dispersive solvent type and amount, pH, and salt effect that affect extraction output. The limits of detection and quantification of the developed method were between 0.09 and 3.36 and 0.31 and 11.19 ng mL, respectively. The calibration plots of the analytes also showed good linearity and low percent relative standard deviations. Recovery studies were performed for tap water and wastewater samples, and the percent recoveries recorded were between 84 and 109%.
Four simple, rapid, and accurate spectrophotometric methods were developed for the simultaneous determination of two food colorants, Carmoisine (E122) and Ponceau 4R (E124), in their binary mixtures and soft drinks. The first method is based on recording the first derivative curves and determining each component using the zero-crossing technique. The second method uses the first derivative of ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The third method, derivative differential procedure, is based on the measurement of difference absorptivities derivatized in first order of solution of drink samples in 0,1 N NaOH relative to that of an equimolar solution in 0,1 N HCl at wavelengths of 366 and 451 nm for Carmoisine and Ponceau 4R, respectively. The last method, based on the compensation method is presented for derivative spectrophotometric determination of E122 and E124 mixtures with overlapping spectra. By using ratios of the derivative maxima, the exact compensation of either component in the mixture can be achieved, followed by its determination. These proposed methods have been successfully applied to the binary mixtures and soft drinks and the results were statistically compared with the reference HPLC method (NMKL 130).
In this study, a switchable solvent was used to preconcentrate trace amounts of Cd from aqueous solution for its determination by flame atomic absorption spectrometry (FAAS). Protonation of N,N-dimethylbenzylamine by dry ice (solid CO) made it water soluble, and addition of sodium hydroxide converted it back to its original nonionic state for phase separation and subsequent extraction of Cd. A slotted quartz tube (SQT) was attached to the flame burner head to increase the residence time of Cd atoms in the light path. Under the optimum conditions, limits of detection and quantification were determined as 0.7 and 2.6 μg L, respectively. Low relative standard deviations calculated from seven replicate measurements of the lowest concentration indicated high precision. Accuracy of the developed method was checked by using a standard reference material (SRM 1633c). Spiked recovery tests were also performed on lake water and wastewater samples at different concentrations to check the applicability of the developed method, and the results obtained (90-103%) established high recovery.
Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue) and two sweeteners (Acesulfame-K and Aspartame) in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS), is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K) and third-derivative curve (for Aspartame) and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS), depends on application ratio spectra of first-and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992-0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 gmL −1 and from 0.06 to 0.47 gmL −1 , respectively. The intraday and interday precision tests produced good RSD% values (<0.81%); recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.
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