Moniruzzaman M, Rodríguez I, Rodríguez-Cabo T, Cela R, Sulaiman S A, Gan S H
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain; Department of Pharmacology, School of Medical Sciences, Universiti Sains Malaysia, Kubang Kerian, Kelantan, 16150 Malaysia.
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
J Chromatogr A. 2014 Nov 14;1368:26-36. doi: 10.1016/j.chroma.2014.09.057. Epub 2014 Sep 30.
The suitability of the dispersive liquid-liquid microextraction (DLLME) technique for gas chromatography (GC) characterization of minor organic compounds in honey samples is evaluated. Under optimized conditions, samples were pre-treated by liquid-liquid extraction with acetonitrile followed by DLLME using carbon tetrachloride (CCl4, 0.075 mL) as extractant. The yielded settled phase was analyzed by GC using high resolution time-of-flight (TOF) mass spectrometry (MS). The whole sample preparation process is completed in approximately 10 min, with a total consumption of organic solvents below 4 mL, relative standard deviations lower than 12% and with more than 70 organic compounds, displaying linear retention index in the range from 990 to 2900, identified in the obtained extracts. In comparison with HS SPME extraction, higher peak intensities were attained for most volatile and semi-volatile compounds amenable to both extraction techniques. Furthermore, other species such as highly polar and water soluble benzene acids, long chain fatty acids, esters and flavonoids, which are difficult to concentrate by HS SPME, could be identified in DLLME extracts. Some of the compounds identified in DLLME extracts have been proposed as useful for samples classification and/or they are recognized as markers of honeys from certain geographic areas.
评估了分散液液微萃取（DLLME）技术用于气相色谱（GC）表征蜂蜜样品中微量有机化合物的适用性。在优化条件下，样品先用乙腈进行液液萃取预处理，然后以四氯化碳（CCl4，0.075 mL）为萃取剂进行DLLME。所得的沉降相通过GC联用高分辨率飞行时间（TOF）质谱（MS）进行分析。整个样品制备过程约需10分钟完成，有机溶剂总消耗量低于4 mL，相对标准偏差低于12%，并且在所获得的提取物中鉴定出70多种有机化合物，其线性保留指数范围为990至2900。与顶空固相微萃取（HS SPME）萃取相比，对于两种萃取技术都适用的大多数挥发性和半挥发性化合物，DLLME获得了更高的峰强度。此外，在DLLME提取物中还可以鉴定出其他一些物质，如高极性和水溶性的苯甲酸、长链脂肪酸、酯类和黄酮类化合物，这些物质难以通过HS SPME进行富集。DLLME提取物中鉴定出的一些化合物已被认为可用于样品分类和/或被视为特定地理区域蜂蜜的标志物。
