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首页> 外文期刊>Environmental toxicology and chemistry >AQUEOUS SAMPLE PREPARATION FOR BIOASSAY USING SUPERCRITICAL FLUID EXTRACTION
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AQUEOUS SAMPLE PREPARATION FOR BIOASSAY USING SUPERCRITICAL FLUID EXTRACTION

机译：超临界流体萃取法制备生物测定用水的样品

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摘要

Supercritical fluid extraction (SFE) has become a valuable tool in the preparation of environmental samples for analysis. Most applications to date have been to extract compounds from solid matrices for later analysis by gas chromatographic or high-performance liquid chromatographic methods. The objective of this research was to extend SFE applications to aqueous samples extracted on Empore~™ (C_(18)) solid-phase extraction disks. This technique, which essentially eliminated the use of conventional solvents in preparing the filtered samples, yielded extracts that were compatible with bioassay. The method included aqueous sample extraction onto C_(18) Empore disks and subsequent elution with supercritical CO_2 to isolate and concentrate analytes of interest, using glass beads as an off-line trapping matrix. Analytes were then redissolved in reconstituted water and evaluated for toxicity using the larval medaka, Oryzias latipes, 96-h static toxicity bioassay. Tests with water spikes of molinate, thiobencarb, methyl parathion, and malathion extracted on disks and eluted by SFE gave quantitative recoveries ( >90%). Samples of a mixture of these compounds prepared using SFE produced an LC50 of 2.88 mg/L, compared with an LC50 of 2.60 mg/L produced by a water sample directly spiked with equivalent concentrations. Extracts of rice-field water prepared for bioassay and gas chromatographic analysis using the SFE method gave good recoveries without loss of biological activity.
机译：超临界流体萃取（SFE）已成为制备环境样品进行分析的重要工具。迄今为止，大多数应用是从固体基质中提取化合物，以通过气相色谱法或高效液相色谱法进行后续分析。这项研究的目的是将SFE应用扩展到在Empore™（C_（18））固相萃取盘上萃取的水性样品中。该技术从根本上消除了在制备过滤样品中使用常规溶剂的作用，从而产生了与生物测定兼容的提取物。该方法包括将水性样品提取到C_（18）Empore圆盘上，然后使用玻璃珠作为离线捕获基质，用超临界CO_2进行洗脱，以分离和浓缩目标分析物。然后将分析物重新溶解在再生水中，并使用幼虫medaka，Oryzias latipes，96小时静态毒性生物测定法评估毒性。在圆盘上提取并用SFE洗脱的水样高岭土，硫代苯甲酸，甲基对硫磷和马拉硫磷的加标品定量回收率（> 90％）。使用SFE制备的这些化合物的混合物样品的LC50为2.88 mg / L，而直接加标等效浓度的水样品的LC50为2.60 mg / L。使用SFE方法制备的用于生物测定和气相色谱分析的稻田水提取物可实现良好的回收率，且不会损失生物活性。

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