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Sensitive determination of glycerol by derivatization using a HPLC-DAD method in biodiesel samples

机译:HPLC-DAD法衍生化测定生物柴油样品中的甘油

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摘要

Biodiesel is mainly produced through a transesterification reaction which yields biodiesel and glycerol, a byproduct. This article describes the quantification of glycerol based on high performance liquid chromatography (HPLC) using a diode array detector (DAD) in various biodiesel samples through post-derivatization. Glycerol was converted into a UV active product i.e. glyceryl tribenzoate (GTB) through a simple and effective esterification reaction using benzoyl chloride and copper chloride as the catalyst under mild conditions. Optimized reaction conditions (affording a 90% yield) were obtained by using copper chloride (17 mol%), benzoyl chloride (12.0 equiv.) and triethyl amine (11.0 equiv.). The limit of detection and limit of quantification were found to be 0.23 mu g mL(-1) and 0.76 mu g mL(-1), respectively. The developed and validated HPLC-DAD method is sensitive, selective, reproducible and successfully applied for the quantification of glycerol in biodiesel from various sources.
机译:生物柴油主要通过酯交换反应生产,该反应会产生生物柴油和副产物甘油。本文介绍了基于高效液相色谱(HPLC)的甘油的定量方法,该方法使用衍生化后的二极管阵列检测器(DAD)对各种生物柴油样品中的甘油进行定量。在温和的条件下,使用苯甲酰氯和氯化铜作为催化剂,通过简单有效的酯化反应,将甘油转化为UV活性产物,即三苯甲酸甘油酯(GTB)。通过使用氯化铜(17摩尔%),苯甲酰氯(12.0当量)和三乙胺(11.0当量)获得了最佳的反应条件(产率为90%)。检出限和定量限分别为0.23μg mL(-1)和0.76μg mL(-1)。经过开发和验证的HPLC-DAD方法灵敏,选择性强,可重现,并成功地用于各种来源生物柴油中甘油的定量分析。

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