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Detection of trans-fatty acids by high performance liquid chromatography coupled with in-tube solid-phase microextraction using hydrophobic polymeric monolith

机译:使用疏水聚合物整体用高效液相色谱法检测高效液相色谱法与管式固相微萃取的高效液相色谱法

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Based on in-tube solid-phase microextraction (in-tube SPME) using a hydrophobic poly (octadecyl methacrylate-co-ethylene dimethacrylate) [poly (OMA-co-EDMA)] monolith, a simple high performance liquid chromatography (HPLC) method has been developed for detection of trans-fatty acids (TFAs) as their fatty acid methyl esters (FAMEs). The poly (OMA-co-EDMA) monolithic column with high hydrophobicity was specially prepared for simultaneous microextraction, pre-separation and purification for the analytes. The pre-separation selectivity, the extraction efficiency, and the purification effect for FAMEs were investigated respectively. Furthermore, some operation parameters have been optimized in detail with respect to satisfactory extraction efficiency of the target compounds. Under the optimized conditions, the enrichment factors for model FAMEs were ranged from 58.3 to 70.9, wide linear range (0.01-1.00 mg/kg) and low detection limits (LODs) (3.0-7.1 mu g/kg) were achieved, respectively. In addition, recoveries of the method were in the range from 83.0 to 106.4% with low relative standard deviations (RSDs) of 3.2-4.7% (n =4) at spiking levels of 0.05, 0.25 and 0.5 mg/kg, respectively. Finally, the proposed method was successfully applied for detection of TFAs in practical samples, which possesses short time-consuming, low disturbance and high detection sensitivity. (C) 2016 Elsevier B.V. All rights reserved.
机译:使用疏水性聚(甲基丙烯酸甲酯 - 共乙烯二甲基丙烯酸甲酯)[聚(OMA-Co-EDMA)]整体,一种简单的高效液相色谱(HPLC)方法,基于管式固相微萃取(管道SPME)。已经开发出用于检测转脂酸(TFA)作为其脂肪酸甲酯(FAME)。具有高疏水性的聚(OMA-Co-EDMA)单片柱专门用于同时进行微萃取,分类预分离和纯化。研究分别预分离选择性,提取效率和针对FAME的纯化效果。此外,关于靶向化合物的令人满意的提取效率,已经详细优化了一些操作参数。在优化条件下,模型FAME的富集因子范围为58.3至70.9,分别宽线性范围(0.01-1.00mg / kg)和低检测限(LOD)(3.0-7.1μg/ kg)。此外,该方法的回收率在83.0至106.4%的范围内,相对标准偏差(RSD)分别为0.05,0.25和0.5mg / kg的尖峰水平为3.2-4.7%(n = 4)。最后,在实际样品中成功地应用于检测TFA的方法,该方法具有短耗时,低扰动和高检测灵敏度。 (c)2016年Elsevier B.v.保留所有权利。

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