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Rapid determination of tetrabromobisphenol A and its main derivatives in aqueous samples by ultrasound-dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

机译:超声分散液液微萃取-高效液相色谱法快速测定水性样品中四溴双酚A及其主要衍生物

摘要

A method of ultrasound-dispersive liquid-liquid microextraction (US-DLLME) combined with high-performance liquid chromatography/variable wavelength detection (HPLC-VWD) has been developed for rapid measuring tetrabromobisphenol A and its five derivatives in water. Parameters affecting the extraction efficiency including the extraction solvents and dispersive solvents and their volume, ionic strength of the sample, and ultrasound time were optimized, and further validated by orthogonal array design (OAD). The optimized conditions provided enrichment factors for analytes of 74-490. Most analytes had linear responses between 2 and 500 mu g L-1, with correlation coefficients (r(2)) of 0.9923-0.9994. Limits of detection were 0.13-0.63 mu g L-1. Relative standard deviations (RSDs) for five replicates ranged from 2.6% to 4.5% for all analytes. When applied to spiked samples of real water, the method provided recoveries of 88.6-106.3% for tap water, 87.8-108.5% for Mi River water, 82.7-113.5% for chemical wastewater, 45.5-115.3% for urine, and 46.4-126.2% for fruit juice, with RSDs (n=5) less than 4%, 6%, 8%, 10%, and 9% respectively. (C) 2013 Published by Elsevier B.V.
机译:超声分散液-液微萃取(US-DLLME)与高效液相色谱/可变波长检测(HPLC-VWD)相结合的方法已经开发出来,用于快速测定水中的四溴双酚A及其五种衍生物。优化了影响萃取效率的参数,包括萃取溶剂和分散溶剂及其体积,样品的离子强度和超声时间,并通过正交阵列设计(OAD)进行了进一步验证。优化的条件为74-490的分析物提供了富集因子。大多数分析物的线性响应在2至500μgL-1之间,相关系数(r(2))为0.9923-0.9994。检测限为0.13-0.63μgL-1。对于所有分析物,五次重复的相对标准偏差(RSD)为2.6%至4.5%。当用于加标的真实水样品中时,该方法的自来水回收率为88.6-106.3%,密河水为87.8-108.5%,化学废水为82.7-113.5%,尿液为45.5-115.3%,尿液为46.4-126.2果汁的RSD(n = 5)分别小于4%,6%,8%,10%和9%。 (C)2013由Elsevier B.V.发布

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