Optimization of parameters affecting the recovery in the analysis of polycyclic aromatic hydrocarbons in natural waters by HPLC-fluorescence

Rosa Amaro, Norielys Herrera, Katya Reategui
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Abstract

To improve the recovery percentages in the analysis of PAH (polycyclic aromatic hydrocarbons) in natural waters, parameters such as standard stability, filtration, storage time and matrix effect were optimized for five PAH by HPLC-FD. For aqueous standards, with the addition of 10% acetonitrile, good linearity was found for naphthalene, acenaphthene, anthracene, pyrene, and chrysene curves up to the second day of standards preparation. In filtration, the best results were obtained using the AP10 and Nylon filters with 10% acetonitrile, with recovery ranges of 98-72% and 93-56%, respectively. In contrast, lower values were obtained with cellulose filters in a polyethylene holder without the addition of 10% acetonitrile with recoveries of 52-0%. A 23 factorial design established, for natural water, that the most important factors were: storage time for naphthalene and acenaphthene, with area losses at 48 hours and the use of organic solvent for anthracene, pyrene and chrysene, with area gain for 20 % acetonitrile. For liquid-liquid extraction in standards, recoveries of 62-45% were found in aqueous matrix without acetonitrile and 98-35% with 20% acetonitrile + 2.5% NaCl, at 24 hours of preparation.
用高效液相色谱-荧光法分析天然水体中的多环芳烃时影响回收率的参数的优化
为了提高天然水体中多环芳烃(PAH)分析的回收率,采用 HPLC-FD 对五种多环芳烃的标准品稳定性、过滤、储存时间和基质效应等参数进行了优化。在水性标准品中,加入 10%的乙腈后,萘、苊、蒽、芘和菊烯的曲线在标准品制备的第二天之前都具有良好的线性关系。在过滤过程中,使用 AP10 和尼龙过滤器与 10%的乙腈可获得最佳结果,回收率范围分别为 98-72% 和 93-56%。相比之下,使用聚乙烯支架中的纤维素过滤器,在不添加 10%乙腈的情况下获得的回收率较低,为 52-0%。对天然水进行 23 因子设计后发现,最重要的因素是:萘和苊的储存时间(48 小时后面积损失),以及蒽、芘和菊烯的有机溶剂使用(20% 乙腈的面积增加)。对于标准物质的液液萃取,在水基中不使用乙腈的回收率为 62-45%,使用 20% 乙腈 + 2.5% NaCl 的回收率为 98-35%(制备时间为 24 小时)。
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