School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou, China.
Anal Chem. 2012 Jul 3;84(13):5816-22. doi: 10.1021/ac301274r. Epub 2012 Jun 22.
Microwave accelerated selective Soxhlet extraction (MA-SSE), a novel selective extraction technique, was investigated in this study. A Soxhlet extraction system containing a glass filter was designed as an extractor. During the procedure of MA-SSE, both the target analytes and the interfering components were extracted from the sample into the extraction solvent enhanced by microwave irradiation. After the solvent flowed though the sorbent, the interfering components were adsorbed by the sorbent, and the target analytes remaining in the solvent were collected in the extraction bottle. No cleanup or filtration was required after extraction. The efficiency of the MA-SSE approach was demonstrated in the determination of organophosphorus and carbamate pesticide residues in ginseng by gas chromatography/mass spectrometry (GC/MS). Under the optimized conditions, low limits of detection (0.050-0.50 μg/kg) were obtained. The recoveries were in the range of 72.0-110.1% with relative standard deviations less than 7.1%. Because of the effect of microwave irradiation, MA-SSE showed significant advantage compared with other extraction techniques. The sorbent used in this study showed good cleanup ability. The mechanism of MA-SSE was demonstrated to be based on the rupture of the cell walls according to the structural changes of ginseng samples. On the basis of the results, MA-SSE as a simple and effective sample preparation technique for the analysis of pesticide residues in complex matrixes shows great promise.
微波加速选择性索氏提取(MA-SSE)是一种新颖的选择性提取技术,本研究对此进行了探讨。设计了一种含有玻璃过滤器的索氏提取系统作为提取器。在 MA-SSE 过程中,目标分析物和干扰成分都在微波辐射增强的提取溶剂中从样品中被提取出来。溶剂流经吸附剂后,干扰成分被吸附剂吸附,而留在溶剂中的目标分析物则被收集在提取瓶中。提取后无需进行清洗或过滤。通过气相色谱/质谱法(GC/MS)测定人参中的有机磷和氨基甲酸酯农药残留,证明了 MA-SSE 方法的效率。在优化条件下,检测限低至 0.050-0.50 μg/kg。回收率在 72.0-110.1%之间,相对标准偏差小于 7.1%。由于微波辐射的影响,MA-SSE 与其他提取技术相比具有明显优势。本研究中使用的吸附剂具有良好的净化能力。MA-SSE 的机理被证明是基于细胞壁的破裂,根据人参样品的结构变化。基于这些结果,MA-SSE 作为一种简单有效的样品制备技术,用于分析复杂基质中的农药残留,具有广阔的前景。