High-Performance Liquid Chromatography Using Ultraviolet Detection for Separation of Terephthalic Acid and Associated Impurities from Recycled Materials.

IF 1.5 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS
Mehdi Ashraf-Khorassani, William M Coleman Iii, Tripp Aardema
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Abstract

An optimized rapid and precise high-performance liquid chromatography method has been developed to separate, identify and quantitate impurities contained within terephthalic acid (TPA) produced from recycled materials. Using a Waters X-Select HSS T3 column for the separation of recycled TPA and eight impurities, and a mobile phase of H2O/CH3CN containing 0.1% trifluoroacetic acid (TFA) with detection by UV at 250 nm, baseline separation of all compounds was achieved in ˂17 min. Four different mobile phase acidic additives were tested, the results indicating that mobile phases with lower pH provided better separation of the compounds with accompanying improved peak shapes. Among all the acidic additives tested in this study, a mobile phase containing 0.1% TFA demonstrated the highest resolution and the best peak shapes. It was concluded that by suppressing the ionization of the acidic compounds contained in the samples through increased acidity of the mobile phase, better peak shapes and higher resolution could be achieved. The amount of increased mobile phase acidity was based in part on the pKa values of the analytes and adjusted so as to eliminate as much as possible any dissociation of the organic acids. A comparison of a standard addition method versus an external calibration curve approach for the quantification of impurities showed similar results, even for relatively low-concentration analytes at levels below 10 ppm. The aspects often linked with validated analytical methods were addressed including linearity, limit of detection, limit of quantitation, sensitivity and selectivity, addressing the criteria set forth in the acronyms of the QuECHERS method description, that is quick easy, cheap, effective, rugged and safe.

紫外检测高效液相色谱法分离回收材料中对苯二甲酸及其伴生杂质。
建立了一种优化的快速、精确的高效液相色谱法,用于分离、鉴定和定量回收材料生产的对苯二甲酸(TPA)中的杂质。采用Waters X-Select HSS T3色谱柱对回收的TPA和8种杂质进行分离,以含有0.1%三氟乙酸(TFA)的H2O/CH3CN为流动相,在250 nm波长下进行紫外检测,所有化合物的基线分离时间为小于17 min。对四种不同的酸性流动相添加剂进行了测试,结果表明,pH较低的流动相可以更好地分离化合物,并改善了峰形。在本研究测试的所有酸性添加剂中,含有0.1% TFA的流动相具有最高的分辨率和最佳的峰形。结果表明,通过增加流动相的酸度来抑制样品中酸性化合物的电离,可以获得更好的峰形和更高的分辨率。流动相酸度的增加部分基于分析物的pKa值,并进行调整,以尽可能多地消除有机酸的解离。标准添加法与外部校准曲线法在杂质定量方面的比较显示出相似的结果,即使对于低于10ppm的相对低浓度分析物也是如此。解决了通常与验证分析方法相关的方面,包括线性,检测限,定量限,灵敏度和选择性,解决了QuECHERS方法描述中首字母缩略词中规定的标准,即快速,简单,廉价,有效,坚固和安全。
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来源期刊
CiteScore
2.90
自引率
7.70%
发文量
94
审稿时长
5.6 months
期刊介绍: The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.
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