Abdel-Aziz Omar, El Kosasy A M, El-Sayed Okeil S M
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain-Shams University, Cairo, Egypt.
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ain-Shams University, Cairo, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2014 Dec 10;133:119-29. doi: 10.1016/j.saa.2014.05.059. Epub 2014 May 29.
A modified dispersive liquid-liquid extraction (DLLE) procedure coupled with spectrophotometric techniques was adopted for simultaneous determination of naphthalene, anthracene, benzo(a)pyrene, alpha-naphthol and beta-naphthol in water samples. Two different methods were used, partial least-squares (PLS) method and a new derivative ratio method, namely extended derivative ratio (EDR). A PLS-2 model was established for simultaneous determination of the studied pollutants in methanol, by using twenty mixtures as calibration set and five mixtures as validation set. Also, in methanol a novel (EDR) method was developed for determination of the studied pollutants, where each component in the mixture of the five PAHs was determined by using a mixture of the other four components as divisor. Chemometric and EDR methods could be also adopted for determination of the studied PAH in water samples after transferring them from aqueous medium to the organic one by utilizing dispersive liquid-liquid extraction technique, where different parameters were investigated using a full factorial design. Both methods were compared and the proposed method was validated according to ICH guidelines and successfully applied to determine these PAHs simultaneously in spiked water samples, where satisfactory results were obtained. All the results obtained agreed with those of published methods, where no significant difference was observed.
采用改进的分散液液萃取（DLLE）方法结合分光光度技术，同时测定水样中的萘、蒽、苯并(a)芘、α-萘酚和β-萘酚。使用了两种不同的方法，即偏最小二乘法（PLS）和一种新的导数比方法，即扩展导数比（EDR）。通过使用二十个混合物作为校准集和五个混合物作为验证集，建立了PLS-2模型，用于同时测定甲醇中所研究的污染物。此外，在甲醇中开发了一种新颖的（EDR）方法来测定所研究的污染物，其中五种多环芳烃混合物中的每种成分通过使用其他四种成分的混合物作为除数来测定。通过利用分散液液萃取技术将水样从水相介质转移到有机相后，化学计量学和EDR方法也可用于测定水样中所研究的多环芳烃，其中使用全因子设计研究了不同参数。对这两种方法进行了比较，并根据国际协调会议（ICH）指南对所提出的方法进行了验证，该方法成功应用于同时测定加标水样中的这些多环芳烃，获得了满意的结果。所有获得的结果与已发表方法的结果一致，未观察到显著差异。
