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Separation of Aliphatic and Aromatic Carboxylic Acids by Conventional and Ultra High Performance Ion Exclusion Chromatography

机译:常规和超高效离子排斥色谱法分离脂肪族和芳香族羧酸

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摘要

An ion exclusion chromatography (IELC) comparison between a conventional ion exchange column and an ultra-high performance liquid chromatography (UHPLC) dynamically surfactant modified C18 column for the separation of an aliphatic carboxylic acid and two aromatic carboxylic acids is presented. Professional software is used to optimize the conventional IELC separation conditions for acetylsalicylic acid and the hydrolysis products: salicylic acid and acetic acid. Four different variables are simultaneously optimized including H2SO4 concentration, pH, flow rate, and sample injection volume. Thirty different runs are suggested by the software. The resolutions and the time of each run are calculated and feed back to the software to predict the optimum conditions. Derringer’s desirability functions are used to evaluate the test conditions and those with the highest desirability value are utilized to separate acetylsalicylic acid, salicylic acid, and acetic acid. These conditions include using a 0.35 mM H2SO4 (pH 3.93) eluent at a flow rate of 1 mL min-1 and an injection volume of 72 μL. To decrease the run time and improve the performance, a UHPLC C18 column is used after dynamic modification with sodium dodecyl sulfate. Using pure water as a mobile phase, a shorter analysis time and better resolution are achieved. In addition, the elution order is different from the IELC method which indicates the contribution of the reversed-phase mode to the separation mechanism.
机译:进行了常规离子交换柱与超高效液相色谱(UHPLC)动态表面活性剂修饰的C18柱之间的离子排斥色谱(IELC)比较,该色谱用于分离脂肪族羧酸和两种芳族羧酸。使用专业软件优化乙酰水杨酸和水解产物(水杨酸和乙酸)的常规IELC分离条件。同时优化了四个不同的变量,包括H2SO4浓度,pH,流速和进样量。该软件建议进行三十次不同的运行。计算每次运行的分辨率和时间,并将其反馈给软件以预测最佳条件。 Derringer的合意函数用于评估测试条件,而合意值最高的函数用于分离乙酰水杨酸,水杨酸和乙酸。这些条件包括使用0.35 mM H2SO4(pH 3.93)洗脱液,流速为1 mL min -1 ,进样量为72μL。为了减少运行时间并提高性能,在用十二烷基硫酸钠动态修饰后使用UHPLC C18色谱柱。使用纯水作为流动相,可以缩短分析时间并提高分离度。此外,洗脱顺序与IELC方法不同,IELC方法表明反相模式对分离机理的贡献。

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