Li Yizhe, Bao Guirong, Wang Hua
Faculty of Materials and Metallurgical Engineering, Kunming University of Science and Technology, Kunming 650093, China.
Se Pu. 2008 Jul;26(4):494-8. doi: 10.1016/s1872-2059(08)60025-5.
A method for the determination of 11 familiar components in biodiesel was developed using ultra performance liquid chromatography with evaporative light scattering detector (UPLC-ELSD). These components were oleic acid, methyl cis-9-octadecenoate, linoleic acid, methyl linoleate, stearic acid, methyl octadecanoate, methyl linolenate, palmitic acid, methyl hexadecanoate, erucic acid and myristic acid. The sample was dissolved in methanol after extraction from the products. The separation column was an Acquity UPLC BEH Phenyl C18 (100 mm x 2.1 mm, 1.7 microm) and the mobile phase was acetonitrile-water (3:1, v/v). An isocratic elution program was utilized for the separation. The flow rate was 0.3 mL/min and the column temperature was 40 degrees C. The parameters of ELSD were as follows: the plus was 80; the temperature of the drift tube was 45 degrees C; the eluant gas pressure was 172 kPa. The sample was detected by ELSD in only 5 min. The calibration curves of 11 components showed good linearity with the correlation coefficients greater than 0.997. In comparison with other methods, this method is simple, fast, and has a good separation efficiency. The fatty acids and fatty acid methyl esters were separated in one step, thus, the extent of reaction can be confirmed by the determination of their contents. This method can be routinely used for the determination of the fatty acids and fatty acid methyl esters in the reaction products and the final biodiesel.
建立了一种采用超高效液相色谱-蒸发光散射检测器(UPLC-ELSD)测定生物柴油中11种常见成分的方法。这些成分包括油酸、顺-9-十八碳烯酸甲酯、亚油酸、亚油酸甲酯、硬脂酸、十八烷酸甲酯、亚麻酸甲酯、棕榈酸、十六烷酸甲酯、芥酸和肉豆蔻酸。样品从产物中萃取后溶于甲醇。分离柱为Acquity UPLC BEH苯基C18(100 mm×2.1 mm,1.7μm),流动相为乙腈-水(3:1,v/v)。采用等度洗脱程序进行分离。流速为0.3 mL/min,柱温为40℃。蒸发光散射检测器的参数如下:增益为80;漂移管温度为45℃;洗脱气体压力为172 kPa。样品仅需5分钟即可通过蒸发光散射检测器进行检测。11种成分的校准曲线具有良好的线性,相关系数大于0.997。与其他方法相比,该方法简单、快速,分离效率良好。脂肪酸和脂肪酸甲酯一步分离,因此,通过测定其含量可确定反应程度。该方法可常规用于测定反应产物和最终生物柴油中的脂肪酸及脂肪酸甲酯。