Abstract
Dispersive liquid--liquid microextraction followed by a back-extraction step was combined with HPLC-DAD for the determination of four parabens (i.e. methyl-, ethyl-, propyl-, and butylparaben). Optimum extraction conditions were found as follows: 225 $\mu $L of chloroform, 0.75 mL of ethanol, 7.5 mL of aqueous solution and within an extraction time of 15 s. Back-extraction into 100 $\mu $L of 50 mM sodium hydroxide solution within 20 s resulted in a reversed-phase HPLC-compatible extract. The analytes were separated at 20 $^{\circ}$C using methanol (A) and water (B), 40:60 (A:B, v/v) as the mobile phase, a flow rate of 1.0 mL min$^{-1}$ and an injection volume of 20 $\mu $L. DAD was set at 258 nm to monitor the analytes. Limits of detection and quantitation were as low as 0.1 and 0.3 $\mu $g mL$^{-1}$, respectively. Coefficients of determination (R$^{2})$ were higher than 0.9950 and percentage relative recoveries were found in the range of 86.5-114.5% for the four parabens from pharmaceuticals and personal care products.
Highlights
Esters of p -hydroxybenzoic acid, or parabens, are extensively employed as preserving agents in a large number of processed food, pharmaceuticals and personal care products (PCPs) including creams, body lotions, mouth rinses, toothpastes, and shampoos
dispersive liquid-liquid microextraction (DLLME)-HPLC-diode-array detector (DAD) is proposed for quantitation of the four parabens in pharmaceuticals and PCPs with a main focus on minimizing the extraction time and organic solvents without derivatization
Dilution of the samples was adopted for the aftershave cream, mouth rinse and baby cream, whereas solid-liquid extraction (SLE) into EtOH was applied for wipes
Summary
Esters of p -hydroxybenzoic acid, or parabens, are extensively employed as preserving agents in a large number of processed food, pharmaceuticals and personal care products (PCPs) including creams, body lotions, mouth rinses, toothpastes, and shampoos. Due to the complexity of these matrices, applying an extraction step like liquid–liquid extraction (LLE) or solid-phase extraction (SPE) was necessary prior to separation and/or detection [11,12] These traditional extraction methods require significant amounts of the sample and toxic organic solvents, and the applied procedures are rather long, making them labor-intensive, cost-ineffective, and environmentally unfriendly [13]. DLLME has drawn much attention as an outstanding technique that offers simple and cost-effective extraction of analytes within a short time [17] The novelty of this method relies on the rapid injection of a water-miscible disperser solvent into the donor phase to disperse the water-immiscible organic acceptor phase. DLLME-HPLC-DAD is proposed for quantitation of the four parabens in pharmaceuticals (antacid suspension, antiinflammatory solution, and anticough syrup) and PCPs (aftershave cream, baby cream, mouth rinse, and wet wipes) with a main focus on minimizing the extraction time and organic solvents without derivatization.
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