Cai Jibao, Gao Yun, Zhu Xiaolan, Su Qingde
Department of Chemistry, University of Science & Technology of China, Hefei, 230026, PR China.
Anal Bioanal Chem. 2005 Nov;383(5):869-74. doi: 10.1007/s00216-005-0076-8. Epub 2005 Nov 5.
A novel method combining matrix solid phase dispersion (MSPD) with Soxhlet simultaneous extraction clean-up (SSEC) was developed. Being a single-step extraction and clean-up procedure, it could be used instead of multistep solvent extraction and Florisol column clean-up. It not only reduces sample contamination during the procedure, but it also decreases the amount of organic solvent needed. The retention times of standards were used to qualitatively assess the method, and the external standard method was used to quantitatively assess it. Residues of organochlorine pesticides (OCP) in tobaccos were determined by gas chromatography-electron capture detection (GC-ECD), and their identities were confirmed by the standard addition method (SAM). The performance of the method was evaluated and validated: the detection limit was 0.01-0.02 microg g(-1), relative standard deviations were 5-26%, and recoveries were 72-99% at fortification levels of 0.10, 1.00 and 10.0 microg g(-1). The analytical characteristics of MSPD-SSEC compared very favorably with the results from the classical multistep solvent extraction and Florisol column clean-up method.
开发了一种将基质固相分散（MSPD）与索氏同时萃取净化（SSEC）相结合的新方法。作为一种单步萃取和净化程序，它可用于替代多步溶剂萃取和弗罗里硅土柱净化。它不仅减少了程序中的样品污染，还减少了所需有机溶剂的量。使用标准品的保留时间对该方法进行定性评估，并使用外标法进行定量评估。采用气相色谱 - 电子捕获检测（GC - ECD）测定烟草中有机氯农药（OCP）的残留量，并通过标准加入法（SAM）确认其身份。对该方法的性能进行了评估和验证：检测限为0.01 - 0.02 μg g⁻¹，相对标准偏差为5 - 26%，在0.10、1.00和10.0 μg g⁻¹的加标水平下回收率为72 - 99%。MSPD - SSEC的分析特性与经典的多步溶剂萃取和弗罗里硅土柱净化方法的结果相比非常有利。
