Gonçalves Filho Luiz Carlos, Micke Gustavo Amadeu
Departamento de Química, Universidade Federal de Santa Catarina, CEP 88040-900, Campus Universitário Trindade, Florianópolis, SC, Brazil.
J Chromatogr A. 2007 Jun 22;1154(1-2):477-80. doi: 10.1016/j.chroma.2007.04.063. Epub 2007 May 1.
In this study, a capillary electrophoresis (CE) methodology for the determination of free glycerol in biodiesel using oxidative cleavage with periodate was optimized and validated. The amount of iodate produced in the reaction was determined by CE. The optimized electrolyte was 20 mmol L(-1) glycine and 10 mmol L(-1) trifluoroacetic acid (direct UV detection, 210 nm). The short total analysis time (less than 28 s) was obtained using the short end injection mode. The optimization of the method was carried out using Peakmaster software. The choice of the components of the run electrolyte and of the internal standard (nitrate) was made through the use of effective mobility curves. A good correlation coefficient higher than 0.9991 and low LOD 4.3 mg L(-1) was obtained. The recovery of free glycerol was 95.4-102.4%. This method was used to determine glycerol in commercial biodiesel samples.
在本研究中,对一种使用高碘酸盐氧化裂解来测定生物柴油中游离甘油的毛细管电泳(CE)方法进行了优化和验证。通过CE测定反应中产生的碘酸盐量。优化后的电解质为20 mmol L⁻¹甘氨酸和10 mmol L⁻¹三氟乙酸(直接紫外检测,210 nm)。采用短端进样模式可获得较短的总分析时间(小于28秒)。使用Peakmaster软件对该方法进行了优化。通过有效淌度曲线选择运行电解质和内标(硝酸盐)的成分。获得了高于0.9991的良好相关系数和4.3 mg L⁻¹的低检测限。游离甘油的回收率为95.4 - 102.4%。该方法用于测定商业生物柴油样品中的甘油。