Matrix solid phase dispersion-Soxhlet simultaneous extraction clean-up for determination of organochlorine pesticide residues in tobacco.
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.
Cai
Jibao
J
Department of Chemistry, University of Science & Technology of China, Hefei, 230026, PR China. qdsu@ustc.edu.cn
Gao
Yun
Y
Zhu
Xiaolan
X
Su
Qingde
Q
D005591:Chemical Fractionation / Q000379:methods*; D002849:Chromatography, Gas / Q000379:methods*; D004785:Environmental Pollutants / Q000032:analysis; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D044367:Phase Transition; D010936:Plant Extracts / Q000032:analysis*; D018515:Plant Leaves / Q000737:chemistry*; D011208:Powders; D014026:Nicotiana / Q000737:chemistry*
D004785:Environmental Pollutants; D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D010936:Plant Extracts; D011208:Powders