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Determination of Phthalate Plasticisers in Palm Oil Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC)

机译:使用在线固相萃取 - 液相色谱法测定棕榈油中邻苯二甲酸酯增塑剂(SPE-LC)

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摘要

Contamination of phthalates plasticisers to food has raised concern as some of the phthalates are suspected to be endocrine disruptors. The phthalates have high affinity with oily environment and analysing these chemicals in such matrices is difficult because of the trace amount of the analyte and interference from matrix. An online solid phase extraction (SPE) technique using a large volume (3.5 mL) injection was developed for the analysis of 6 common plasticisers in palm oil. A simple sample preparation involving alumina as a fat retainer and methanol : acetonitrile (1 : 1) as the extraction solvent was performed prior to the usage of online SPE-LC system. This system consists of two columns, C16 for the solid phase extraction (SPE) and C18 as the analytical column, and a photo diode array detector. The calibration curves were linear from 5 to 1000 μg L−1, with correlation coefficients above 0.99. The instrumental limit of detection was 3 μg L−1 and satisfactory recovery was obtained. A screening on a few samples in the retail market revealed the presence of dibutyl phthalate (DBP) and butylbenzylphthalate (BBP) in the palm oil, with concentration less than 1 mg L−1.
机译:邻苯二甲酸酯增塑剂对食物的污染提出了关注,因为一些邻苯二甲酸酯被怀疑是内分泌破坏剂。邻苯二甲酸酯对油性环境具有高亲和力,并且由于痕量的分析物和来自基质的干扰而难以分析这些基质中的这些化学物质。使用大体积(3.5mL)注射的在线固相提取(SPE)技术用于分析棕榈油中的6个常见增塑剂。在使用在线SPE-LC系统之前,进行含有氧化铝作为脂肪固定剂和甲醇的简单样品制备:乙腈(1:1)作为萃取溶剂进行。该系统由两列C16组成,用于固相提取(SPE)和C18作为分析柱,以及光二极管阵列检测器。校准曲线是线性的5至1000μgL-1,其相关系数高于0.99。检测的乐器极限为3μgL-1,并获得令人满意的恢复。零售市场中少数样品的筛选揭示了棕榈油中邻苯二甲酸二丁酯(DBP)和丁基苄基苯二甲酸丁酯(BBP)的存在,浓度小于1mg L-1。

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