Regueiro Jorge, Llompart Maria, Garcia-Jares Carmen, Garcia-Monteagudo Juan C, Cela Rafael
Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentarios, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
J Chromatogr A. 2008 May 9;1190(1-2):27-38. doi: 10.1016/j.chroma.2008.02.091. Epub 2008 Mar 5.
The analytical use of ultrasound-generated emulsions has recently found a growing interest to improve efficiency in liquid-liquid extraction since they increase the speed of the mass transfer between the two immiscible phases implied. Thus, dispersed droplets can act as efficient liquid-liquid microextractors in the continuous phase, and later they can be readily separated by centrifugation. A novel method based on ultrasound-assisted emulsification-microextraction (USAEME) and gas chromatography coupled to mass spectrometry (GC/MS) has been developed for the analysis of synthetic musk fragrances, phthalate esters and lindane in water samples. Extraction conditions were optimized using a multivariate approach. Compounds were extracted during 10 min in an acoustically emulsified media formed by 100 microL chloroform and 10 mL sample (enrichment factor=100). The method performance was studied in terms of accuracy (recovery=78-114%), linearity (R2> or =0.9990) and repeatability (RSD< or =14%). Limits of detection (LODs) were at the pg mL(-1) level for most of compounds, and at the sub-ng mL(-1) level for the most ubiquitous phthalate esters. USAEME is proposed as an efficient, fast, simple and non-expensive alternative to other extraction techniques such as SPE, SPME and LPME for the analysis of environmental waters including bottled, tap, river, municipal swimming pool, sewage and seaport water samples. Since no matrix effect has been found for any of the water types analyzed, quantification could be carried out by using conventional external calibration, thus allowing a higher throughput of the analysis in comparison with other microextraction techniques based on equilibrium such as solid-phase microextraction.
超声产生乳液的分析应用最近越来越受到关注，旨在提高液-液萃取效率，因为它们提高了所涉及的两个不混溶相之间的传质速度。因此，分散的液滴可作为连续相中的高效液-液微萃取器，随后可通过离心轻松分离。已开发出一种基于超声辅助乳化微萃取（USAEME）和气相色谱-质谱联用（GC/MS）的新方法，用于分析水样中的合成麝香香料、邻苯二甲酸酯和林丹。采用多变量方法优化了萃取条件。在由100 μL氯仿和10 mL样品形成的声学乳化介质中萃取10分钟（富集因子=100）。从准确度（回收率=78-114%）、线性（R2≥0.9990）和重复性（RSD≤14%）方面研究了该方法的性能。大多数化合物的检测限（LOD）为pg mL-1水平，最常见的邻苯二甲酸酯的检测限为亚ng mL-1水平。对于包括瓶装水、自来水、河水、市政游泳池水、污水和海港水样在内的环境水样分析，USAEME被认为是一种高效、快速、简单且廉价的替代其他萃取技术（如固相萃取、固相微萃取和液相微萃取）的方法。由于在所分析的任何一种水样中均未发现基质效应，因此可通过常规外部校准进行定量，与其他基于平衡的微萃取技术（如固相微萃取）相比，从而实现更高的分析通量。
