Faculty of Arts and Sciences, Department of Chemistry, Bülent Ecevit University, Zonguldak, Turkey.
J Sep Sci. 2018 Jul;41(13):2750-2758. doi: 10.1002/jssc.201800235. Epub 2018 May 14.
An analytical method is presented for the determination of paraben preservatives in semisolid cream samples by matrix solid-phase dispersion combined with supramolecular solvent-based microextraction. Due to the oily and sticky nature of the sample matrix, parabens were first extracted from the samples by matrix solid-phase dispersion using silica as sorbent material with a clean-up performed with tetrahydrofuran in the elution step. The eluate (500 μL), 1-decanol (120 μL), and water (4.4 mL) were then mixed in a polyethylene pipette to form supramolecular solvent. Finally, the analytes in the supramolecular solvent were separated and determined by liquid chromatography with ultraviolet detection. Under optimal extraction conditions, the extraction recoveries of the studied compounds were obtained in the range of 63-83%. The limits of detection for the analytes were between 0.03 and 0.04 μg/g. The precision of the method varied between 4.0-6.7 (intraday) and 6.2-7.9% (interday). Finally, the optimized procedure was applied to the determination of the target preservatives in a variety of cream samples (diaper rash, skin allergy, face and hand moisturizing) with satisfactory recoveries (86-102%).
本文提出了一种通过基质固相分散结合超分子溶剂基微萃取测定半固体制剂样品中防腐剂的分析方法。由于样品基质的油性和粘性,首先使用硅胶作为吸附剂通过基质固相分散从样品中提取防腐剂,在洗脱步骤中用四氢呋喃进行净化。然后将洗脱液(500 μL)、1-癸醇(120 μL)和水(4.4 mL)在聚乙烯移液管中混合形成超分子溶剂。最后,通过带有紫外检测的液相色谱法分离和测定超分子溶剂中的分析物。在最佳萃取条件下,研究化合物的萃取回收率在 63-83%范围内。分析物的检出限在 0.03 和 0.04 μg/g 之间。该方法的精密度在日内变化为 4.0-6.7%,日间变化为 6.2-7.9%。最后,优化后的方法应用于各种乳膏样品(尿布疹、皮肤过敏、面部和手部保湿)中目标防腐剂的测定,回收率令人满意(86-102%)。