Flores Gema, Blanch Gracia Patricia, Ruiz del Castillo Maria Luisa
Instituto de Fermentaciones Industriales CSIC, Madrid, Spain.
J Sep Sci. 2008 Apr;31(6-7):1207-14. doi: 10.1002/jssc.200700614.
A fully automated method for the determination of medium volatility compounds in aromatic samples was developed. Specifically, the determination of methyl jasmonate in jasmine fragrances was performed by using the through oven transfer adsorption-desorption (TOTAD) interface for the on-line coupling between RPLC-GC. A study of the most relevant variables involved in the performance of the TOTAD interface for medium volatility compounds was carried out by testing different values of helium flow (100, 300, 400, and 500 mL/min), transfer speed (0.1, 0.3, 0.5, and 2.0 mL/min), and methanol/water percentages (86:14, 85:15, 83:17, 80:20, and 70:30). The method developed provided satisfactory repeatability (RSD for retention times of 0.15% and for peak areas of 9.4%) and recovery (71%) as well as excellent LOD (0.01 mg/L) for methyl jasmonate in commercial jasmine essence under the experimental conditions selected as optimum. Additional advantages of the automated RPLC-TOTAD-GC method proposed in the present work are its rapidness, reliability, and the possibility of directly introducing the sample with no further pretreatment.
开发了一种用于测定芳香族样品中中等挥发性化合物的全自动方法。具体而言,通过使用直通式炉转移吸附-解吸(TOTAD)接口实现反相液相色谱-气相色谱(RPLC-GC)在线联用,对茉莉香精中的茉莉酸甲酯进行测定。通过测试不同的氦气流速(100、300、400和500 mL/min)、转移速度(0.1、0.3、0.5和2.0 mL/min)以及甲醇/水百分比(86:14、85:15、83:17、80:20和70:30),对TOTAD接口测定中等挥发性化合物性能中最相关的变量进行了研究。在所选择的最佳实验条件下,所开发的方法对于市售茉莉香精中的茉莉酸甲酯具有令人满意的重复性(保留时间的相对标准偏差为0.15%,峰面积的相对标准偏差为9.4%)和回收率(71%)以及出色的检测限(0.01 mg/L)。本工作中提出的自动RPLC-TOTAD-GC方法的其他优点包括其快速性、可靠性以及无需进一步预处理即可直接进样的可能性。