Coffee is one of the most widely consumed beverages in the world. It contains many bioactive compounds, including chlorogenic acid which possesses various biological properties. In this study, in order to determine concentration of chlorogenic acid in green coffee, a reverse-phase rapid resolution liquid chromatography (RP-RRLC) method with diode-array detection (DAD) was developed. Successful separation was achieved on a Poroshell 120 EC-C18 (50 mm × 3 mm; 2.7 μm) column using acetonitrile–water with 1% phosphoric acid (10:90, v/v) as a mobile phase, at a flow rate of 1 mL/min, and with UV detection at 325 nm. The identification was made with comparison of the retention time of pure analytical standard with the retention time of chlorogenic acid in the analyzed samples. The developed method was validated using the following parameters: linearity, sensitivity, selectivity, precision, and accuracy. Excellent linearity over the range 12.33–143.50 μg/mL was achieved with R2 values greater than 0.99. The intra-day precision was validated with the %RSD values, which confirmed that the method for determination of chlorogenic acid was repeatable. The mean recovery rate of the method ranged between 97.87% and 106.67% with %RSD values lower than 1%. The limit of detection and limit of quantification values under the used chromatographic conditions were 0.29 and 0.96 pg, respectively. This method was successfully employed for quantitative determination of chlorogenic acid in green coffee samples.
The quality of pesticide formulations has an impact on the crop safety, environment and human health. Therefore, the development of new analytical methods for the determination of active substances in pesticide formulations in order to control their quality, as well as, their residues in food samples in order to ensure food safety, is always welcome. A new, simple, precise and accurate normal-phase high-performance liquid chromatography (NP-HPLC) method for determination of an active ingredient malathion in the commercial emulsifiable concentrate pesticide product has been developed and validated. The analysis was carried out on a LiChrosorb CN (250 x 4 mm, 5 μm) analytical column using isocratic elution with mobile phase consisted of n-hexane and dichloromethane (80/20, v/v), flow rate of 1 mL/min, constant column temperature at 25 °C and ultraviolet diode-array detection at 220 nm. The obtained values for multiple correlation coefficients (R2 ≥ 0.9990), relative standard deviation of retention times, peak areas and heights (RSD ≤ 1.14%), recoveries ranged from 98.97 to 101.62%, revealed that the developed method has a satisfactory linearity, precision and accuracy. Also, the developed method was successfully applied for determination of malathion residues in apple juice samples, after preliminary sample preparation using solid-phase extraction. Specificity, selectivity, linearity, matrix effect, precision and accuracy were tested in order to validation of this method. The obtained results were in acceptable ranges and indicated that the developed method is suitable for routine determination of malathion in the pesticide formulation, as well as for determination of malathion residues in apple juice samples. The run time of HPLC analysis was about 6 min.
Summary.Reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous determination of sodium benzoate and potassium sorbate in beverages was developed using high speed column. The simple and rapid reverse-phase method for quantitative determination of both preservatives was established on LiChroCART ® Purospher STAR RP-18e (30 mm × 4 mm; 3 μm) column, mobile phase consisted of acetonitrile-phosphate buffer (pH = 3.5) in volume ratio of 8:92 (v/v), flow rate of 1 mL min −1 , ultraviolet (UV) detection at 195 nm for sodium benzoate and 260 nm for potassium sorbate, and constant column temperature at 25 °C. Linearity, precision, accuracy, limit of quantification (LOQ), and limit of detection (LOD) were tested for method validation. Linearity range for sodium benzoate was 6.04-200.27 mg L −1 (R 2 = 0.999) while, for potassium benzoate (R 2 = 0.999), 12.19-406.36 mg L −1 . The RSD values ≤1.03% demonstrate excellent intra-day precision. LOD for sodium benzoate and potassium sorbate was 0.004 and 0.003 mg L −1 , while LOQ was 0.012 and 0.009 mg L −1 , respectively. This method was applied for quantitative determination of investigated preservatives in beverages which were taken from Macedonian markets.
This study presents the development and validation of a new reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous determination of captan, folpet, and metalaxyl residues in table grape samples with ultraviolet-diode array detection (UV-DAD). Successful separation and quantitative determination of analytes was carried out on LiChrospher 60 RP-select B (250 × 4 mm, 5 μm) analytical column. Mixture of acetonitrile-0.1% formic acid in water (65:35, v/v) was used as a mobile phase, with flow rate of 1 mL/min, constant column temperature at 25°C, and UV detection at 220 nm. The target residues were extracted with acetone by ultrasonication, followed by a cleanup using liquid-liquid extraction (LLE) and solid-phase extraction (SPE). The obtained values for multiple correlation coefficients (R 2 > 0.90), relative standard deviation (RSD) of retention times, peak areas and heights (RSD ≤ 2.25%), and recoveries ranging from 90.55% to 105.40%, with RSD of 0.02% to 5.37%, revealed that the developed method has a good linearity, precision, and accuracy for all analytes. Hence, it is suitable for routine determination of investigated fungicides in table grape samples.
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