期刊
ANALYTICA CHIMICA ACTA
卷 649, 期 2, 页码 135-140出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2009.07.028
关键词
Experimental design; Response surface methodology; Phthalic acid esters; Polycyclic musks
A rapid and simple method for the determination of two phthalates and five polycyclic musks in water samples using dispersive liquid-liquid microextraction (DLLME) mated to chemometrics and coupled to GC-MS was developed. Volume of extraction (CCl4) and disperser solvent (MeOH), pH, ionic strength, extraction time, centrifugation time as well as centrifugation speed were optimized in a 2(7-4) Plackett-Burman design. The obtained significant factors were optimized by using a central composite design (CCD) and the quadratic model between the dependent and the independent variables was built. The optimum experimental conditions of the proposed method were: 250 mu L, carbon tetrachloride, 0.62 ml, methanol, 7.5 min centrifugation time, natural pH containing 0% (w/v) NaCl, while keeping centrifugation speed fixed at 4000 rpm. The calculated calibration curves gave high-level linearity for all target analytes with correlation coefficients ranging between 0.9970 and 0.9992. The repeatability and reproducibility of the proposed method, expressed as relative standard deviation, varied between 2.6% to 9.7% and 5.7% to 12.2%, respectively. The obtained LOD values were in the range of 8-63 ng L-1. (C) 2009 Elsevier B.V. All rights reserved.
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