Panagiotou Aikaterini N, Sakkas Vasilios A, Albanis Triantafyllos A
Department of Chemistry, University of Ioannina, Ioannina 45110, Greece.
Anal Chim Acta. 2009 Sep 7;649(2):135-40. doi: 10.1016/j.aca.2009.07.028. Epub 2009 Jul 14.
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 microL 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).
建立了一种快速简便的方法，采用分散液液微萃取（DLLME）结合化学计量学并与气相色谱-质谱联用，用于测定水样中的两种邻苯二甲酸酯和五种多环麝香。在2(7-4) 普拉凯特-伯曼设计中，对萃取剂（CCl4）和分散剂溶剂（MeOH）的体积、pH值、离子强度、萃取时间、离心时间以及离心速度进行了优化。通过中心复合设计（CCD）对获得的显著因素进行了优化，并建立了因变量与自变量之间的二次模型。该方法的最佳实验条件为：250微升四氯化碳、0.62毫升甲醇、7.5分钟离心时间、含0%（w/v）氯化钠的自然pH值，同时将离心速度固定在4000转/分钟。计算得到的校准曲线对所有目标分析物具有高度线性，相关系数在0.9970至0.9992之间。该方法的重复性和再现性，以相对标准偏差表示，分别在2.6%至9.7%和5.7%至12.2%之间变化。获得的检测限（LOD）值在8-63纳克/升范围内。
