Lu Yang, Zhu Yan
Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, China; Zhejiang Textile Testing Research Institute, Hangzhou 310013, China.
Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, China.
Talanta. 2014 Feb;119:430-4. doi: 10.1016/j.talanta.2013.11.022. Epub 2013 Nov 27.
A simple and environmentally friendly sample preparation procedure coupled with gas chromatography-mass spectrometry was developed to assay dimethyl fumarate in textiles and leathers. The sample preparation procedure involved an accelerated solvent extraction (ASE) using water as the extract solvent, followed by the extraction and concentration of dimethyl fumarate from the aqueous solution using vortex-assisted liquid-liquid microextraction (VALLME). The parameters affecting the ASE and VALLME were optimized to achieve the maximum extraction efficiency, and the performance of the developed method was evaluated. Good linearity was observed over the range assayed (0.01-1mg/kg) with a regression coefficient of 0.998. The limit of detection and enrichment factor for the VALLME step were 0.001 mg/kg and 53, respectively. The intra- and inter-day precision were below 8.9%, and the recovery was approximately 84-103%. The as-developed method was successfully applied to textiles and leather samples.
开发了一种简单且环保的样品制备程序，并结合气相色谱-质谱法来测定纺织品和皮革中的富马酸二甲酯。样品制备程序包括使用水作为萃取溶剂的加速溶剂萃取（ASE），然后使用涡旋辅助液-液微萃取（VALLME）从水溶液中萃取和浓缩富马酸二甲酯。对影响ASE和VALLME的参数进行了优化，以实现最大萃取效率，并对所开发方法的性能进行了评估。在所测定的范围内（0.01-1mg/kg）观察到良好的线性，回归系数为0.998。VALLME步骤的检测限和富集因子分别为0.001mg/kg和53。日内和日间精密度均低于8.9%，回收率约为84-103%。所开发的方法成功应用于纺织品和皮革样品。
