Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
J Chromatogr A. 2018 Aug 24;1564:102-109. doi: 10.1016/j.chroma.2018.06.025. Epub 2018 Jun 10.
This study describes the use of a magnetic multi-walled carbon nanotube composite for the preconcentration of nine parabens (methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, phenyl and benzylparaben) from water and urine samples after in situ acetylation. The enriched extracts were obtained by dispersive magnetic solid phase extraction (DMSPE) and analysed by gas chromatography with mass spectrometry (GC-MS). Several parameters affecting the adsorption (extraction time, magnetic material mass and ionic strength) and desorption (desorption solvent nature and volume, and desorption time) DMSPE steps were investigated. Matrix-matched calibration was recommended for quantification of the samples. Linearities in the 0.5-150 ng mL range were obtained, depending on the compound. Under the optimal experimental conditions, the limits of detection ranged between 0.03 and 2.0 ng mL, depending on the sample matrix and the paraben congener. None of the samples analysed contained the above mentioned parabens. The method was validated with two water samples (harbour and wastewater treatment plant) and two urine samples spiked at two concentration levels. Recoveries in the 81-119% range were obtained.
本研究描述了一种磁性多壁碳纳米管复合材料在原位乙酰化后从水样和尿样中预浓缩九种（甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、苯基和苄基）对羟基苯甲酸酯的应用。通过分散磁固相萃取（DMSPE）富集提取物，并通过气相色谱-质谱联用（GC-MS）进行分析。考察了影响吸附（萃取时间、磁性材料质量和离子强度）和解吸（解吸溶剂性质和体积以及解吸时间）DMSPE 步骤的几个参数。建议采用基质匹配校准法对样品进行定量。根据化合物的不同，线性范围在 0.5-150ng/mL 之间。在最佳实验条件下，检出限范围在 0.03-2.0ng/mL 之间，取决于样品基质和对羟基苯甲酸酯同系物。在所分析的样品中均未检出上述对羟基苯甲酸酯。该方法用两个水样（港口和污水处理厂）和两个尿液样品进行了验证，这两个尿液样品分别在两个浓度水平下进行了加标。回收率在 81-119%范围内。
