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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection
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Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection

机译：超声辅助萃取-高效液相色谱-荧光检测法测定环境固体样品中的壬基酚和壬基酚乙氧基化物

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摘要

A simple and rapid analytical method for the determination of nonylphenol (NP) and nonylphenol ethoxylates (NPEOx) in solid environmental samples has been developed. This method combines an ultrasonic-assisted extraction procedure in small columns and an enrichment step onto C18 solid-phase extraction cartridges prior to separation using HPLC with fluorescence detection. Method optimization was carried out using soil samples fortified at different concentration levels (from 0.1 to 100 μg/g). Under optimum conditions, 2 g of soil was placed in small glass columns and extraction was performed assisted by sonication (SAESC) at 45 °C in two consecutive steps of 15 min using a mixture of H2O/MeOH (30/70). The obtained extracts were collected, loaded onto 500 mg C18 cartridges, and analytes were eluted with 3 × 1 ml of methanol and 1 ml of acetonitrile. Finally, sample extracts were evaporated under a nitrogen stream, redissolved in 500 μl H2O/AcN (50/50), and passed though a 0.45 μm nylon filter before final determination by HPLC-FL. The developed procedure allowed to achieve quantitative recoveries for NP and NPEOx, and was properly validated. Finally, the method was applied to the determination of these compounds in soils and other environmental solid samples such as sediments, compost and sludge.
机译：建立了一种测定固体环境样品中壬基酚（NP）和壬基酚乙氧基化物（NPEOx）的简单快速的分析方法。该方法结合了在小柱中的超声辅助萃取程序和在C18固相萃取柱上的富集步骤，然后使用带荧光检测的HPLC进行分离。使用不同浓度水平（0.1至100μg/ g）强化的土壤样品进行方法优化。在最佳条件下，将2 g土壤放入小玻璃柱中，并在45°C的条件下，使用H2O / MeOH（30/70）的混合物，在连续15分钟的两个连续步骤中，通过超声处理（SAESC）进行提取。收集获得的提取物，装入500 mg C18柱中，用3×1 ml甲醇和1 ml乙腈洗脱分析物。最后，样品提取物在氮气流下蒸发，重新溶解在500μlH2O / AcN（50/50）中，并通过0.45μm尼龙滤膜，然后通过HPLC-FL进行最终测定。所开发的程序可实现NP和NPEOx的定量回收，并已得到正确验证。最后，该方法用于测定土壤和其他环境固体样品（例如沉积物，堆肥和污泥）中的这些化合物。

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