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Ultrasound-assisted Emulsification Microextraction-solvent Floating Solidification- Pre-column Derivatization for the Determination of Estrogens in Water Samples

机译:超声辅助乳化微萃取 - 溶剂浮动凝固 - 柱预衍生化,用于测定水样中的雌激素

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The method of ultrasound-assisted surfactant-enhanced emulsification microextraction combined with pre-column derivatization (UAE-SEEME-SFO-PD) was developed to simultaneously extract and determine the estrogens such as estriol (E3), bisphenol A (BPA), 17α-Ethynylestradiol (EE2), estradiol (E2) and nonylphenol (NP) in water samples. Central composite design was employed to investigate the effects of the factors, including emulsifier (Tween 20) volume, extractant (dodecanol) volume, ultrasonic power, ultrasonic time, the amount of derivating agent (paranitrobenzoyl chloride), temperature of derivatization and derivatization time, on the response of analytes. The optimized analytical conditions were obtained by response surface plot as follows: 40μL of Tween 20, 35μL of dodecanol, 62.5 W of ultrasonic power, 15 min of ultrasonic time, 5.0 mg of derivating agent, temperature of derivatization 35°C and derivatization time 2.0 min, with the linear range of 0.02-2.0 mg/L for E3, BPA, EE2 and E2, 0.02-1.0 mg/L for NP, respectively (the correlation coefficients ranging from 0.9950 to 0.9999). Also, the limits of detection were found between 1.06-5.04μg/L. The spiked recoveries of estrogens under different spiked levels (0.02, 0.20 and 1.00 mg/L) for estrogens were in the range of 88.08-117.33%, and the relative standard deviation (RSD) was of 0.75-9.73%. Additionally, the method could be applied to analysis of estrogens in real water samples (collected from upstream and downstream of a reservoir), and the relative recoveries of estrogens under spiked levels (0.05 and 0.50 mg/L) for estrogens in real water samples were in the range of 85.18-124.17% (RSD 0.30-10.71%).
机译:超声辅助表面活性剂的增强的乳化微柱前衍生化相结合的方法(UAE-SeeME所-SFO-PD)中的溶液同时开发以提取并确定雌激素如雌三醇(E3),双酚A(BPA),17α-炔雌醇(EE2),雌二醇(E2)和壬基酚(NP)水样英寸被采用中心复合设计以调查的因素,包括乳化剂的影响(吐温20)的体积,萃取剂(十二烷醇)体积,超声功率,超声时间,求导剂(paranitrobenzoyl氯乙烯),温度的衍生化和衍生化时间的量,上的分析物的响应。由响应面图如下获得的优化的分析条件:40μL吐温20,十二烷醇的35μL,62.5W¯¯超声功率,超声时间15分钟,5.0毫克求导剂的,衍生化35的温度°C和衍生化时间2.0的分钟,用0.02-2.0毫克/升E3,BPA,EE2和E2,0.02-1.0毫克/升NP的线性范围,分别为(相关系数范围从0.9950至0.9999)。此外,1.06-5.04μg/ L之间,发现检测的极限。雌激素在不同添加水平(0.02,0.20和1.00毫克/升)为雌激素加标回收率在88.08-117.33%的范围内,和相对标准偏差(RSD)是含有0.75-9.73%。另外,该方法可以被应用到实际水样的雌激素的分析,并在添加水平(0.05和0.50毫克/升)的雌激素为雌激素的相对回收率实际水样中分别为(从上游和贮存器的下游收集)在85.18-124.17%(RSD 0.30-10.71%)的范围内。

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