Department of Chemistry, Fudan University, No 220, Handan Road, Shanghai 200433, China.
Talanta. 2010 Sep 15;82(4):1181-5. doi: 10.1016/j.talanta.2010.06.037. Epub 2010 Jul 3.
In this work, for the first time, capillary zone electrophoresis (CZE) technique combined with microwave-assisted extraction (MAE) was developed for the fast quantification of chlorogenic acid (CA) in tobacco residues. CA in tobacco residue samples were extracted by MAE technique, and then analyzed by CZE. As a new sample preparation method for tobacco residues, the MAE procedure is optimized, validated and compared with conventional methods including ultrasonic extraction (USE) and reflux extraction (RE). It is found that MAE gives the best result due to the highest extraction efficiency within shortest extraction time (only 4.0 min). Here, CA is determined by CZE based on the calibration curve of its authentic standard. The method linearity, detection limit, precision and recovery are studied. The results show that the combined MAE and CZE method has a linearity (R(2) 0.991, 0.003-0.5 mg ml(-1)), a limit of detection (0.003 mg ml(-1)), a limit of quantification (0.01 mg ml(-1)), good precision (R.S.D.=4.28%) and a finer recovery (89.0%). The proposed method was successfully applied to the analysis of CA in tobacco residue samples. The experiment results have demonstrated that the CZE combined with MAE is a convenient, fast, economical and reliable method for the determination of CA in tobacco residues.
在这项工作中,首次开发了毛细管区带电泳(CZE)技术与微波辅助提取(MAE)相结合的方法,用于快速定量烟草残渣中的绿原酸(CA)。采用 MAE 技术从烟草残渣样品中提取 CA,然后用 CZE 进行分析。作为一种新的烟草残渣样品制备方法,对 MAE 程序进行了优化、验证,并与包括超声提取(USE)和回流提取(RE)在内的常规方法进行了比较。结果发现,MAE 由于在最短的提取时间(仅 4.0 分钟)内具有最高的提取效率,因此效果最佳。在这里,CA 是根据其真实标准品的校准曲线通过 CZE 来确定的。研究了该方法的线性、检测限、精密度和回收率。结果表明,MAE 和 CZE 联合方法具有线性(R²0.991,0.003-0.5 mg ml⁻¹)、检测限(0.003 mg ml⁻¹)、定量限(0.01 mg ml⁻¹)、良好的精密度(RSD=4.28%)和较好的回收率(89.0%)。该方法成功应用于烟草残渣样品中 CA 的分析。实验结果表明,CZE 与 MAE 相结合是一种方便、快速、经济、可靠的测定烟草残渣中 CA 的方法。