Viñas Pilar, Campillo Natalia, Hernández-Pérez Mónica, Hernández-Córdoba Manuel
Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia, Spain.
Anal Chim Acta. 2008 Mar 17;611(1):119-25. doi: 10.1016/j.aca.2008.01.072. Epub 2008 Feb 7.
A comparison of direct immersion solid-phase microextraction (DI-SPME) and stir bar sorptive extraction (SBSE) coupled to liquid chromatography (HPLC) with fluorimetric detection for the rapid analysis of resveratrol isomers is described. For DI-SPME, a polar Carbowax-template resin (CW/TPR) 50mum fiber was the most efficient and optimum extraction conditions were 40 degrees C and an extraction time of 30min, stirring in the presence of 5% (m/v) sodium chloride and 0.07M acetate/acetic acid buffer (pH 6). Desorption was carried out using the static mode for 10min. Linearity was obtained in the 5-150 and 2-150ngmL(-1) ranges for trans- and cis-resveratrol, with detection limits of 2 and 0.5ngmL(-1), respectively. When using SBSE, a polydimethylsiloxane (PDMS) twister provided best extraction by means of a derivatization reaction in the presence of acetic anhydride and potassium carbonate. The same time and temperature were used for the extraction step in the presence of 2.5% (m/v) sodium chloride, and liquid desorption was performed with 150microL of a 50/50 (v/v) acetonitrile/1% (v/v) acetic acid solution in a desorption time of 15min. Linearity was now between 0.5 and 50ngmL(-1) for trans-resveratrol with a detection limit of 0.1ngmL(-1), while cis-resveratrol could not be extracted. The proposed methods were successfully applied to determining the resveratrol isomer content of wine, must and fruit juices.
本文描述了采用直接浸入式固相微萃取（DI-SPME）和搅拌棒吸附萃取（SBSE）结合高效液相色谱（HPLC）及荧光检测法对白藜芦醇异构体进行快速分析的比较。对于DI-SPME，极性的聚乙二醇/模板树脂（CW/TPR）50μm纤维最为高效，最佳萃取条件为40℃、萃取时间30分钟，在5%（m/v）氯化钠和0.07M乙酸盐/乙酸缓冲液（pH 6）存在下搅拌。采用静态模式进行10分钟的解吸。反式和顺式白藜芦醇在5-150和2-150 ng mL⁻¹范围内呈线性，检测限分别为2和0.5 ng mL⁻¹。使用SBSE时，聚二甲基硅氧烷（PDMS）搅拌棒在乙酸酐和碳酸钾存在下通过衍生化反应提供了最佳萃取效果。在2.5%（m/v）氯化钠存在下，萃取步骤采用相同的时间和温度，并用150μL 50/50（v/v）乙腈/1%（v/v）乙酸溶液进行15分钟的液相解吸。现在反式白藜芦醇在0.5至50 ng mL⁻¹之间呈线性，检测限为0.1 ng mL⁻¹，而顺式白藜芦醇无法被萃取。所提出的方法成功应用于葡萄酒、葡萄汁和果汁中白藜芦醇异构体含量的测定。
