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Chemometrics assisted dispersive liquid-liquid microextraction for quantification of seven UV filters in urine samples by HPLC-DAD

机译:化学计量学辅助的分散液-液微萃取,用于通过HPLC-DAD定量分析尿液样品中的七个紫外线过滤器

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摘要

In the present study, dispersive liquid-liquid microextraction followed by high performance liquid chromatography-diode array detection has been developed as simple, rapid, accurate, and efficient sample preparation method for simultaneous determination of seven organic UV filters in urine samples. The influence of the main effects as well as their interactions was studied through a 2~((6-2)) fractional factorial design. The candidate parameters were: type and volume of dispersant and extraction solvents, sample pH, and salt concentration. Under final optimal conditions, the analytes were extracted from 5 mL of samples by addition of 0.5 mL of acetonitrile (dispersing solvent) containing 70 μL of carbon tetrachloride (extraction solvent), without modifying the pH of the solution and applying the (+1) level of salt concentration (10% w/v NaCl). The assay was linear (R~2 > 0.997), relative recoveries ranged from 86.9 up to 97.3% and the LOQs between 3 and 45 ng mL~(-1) were obtained. The intra-and interday RSDs were lower than 5 and 8% at the middle point of the linear range, respectively. The proposed method was successfully applied to different volunteer urine samples and it was shown that the extraction efficiency was not affected by the type of urine samples.
机译:在本研究中,分散液-液微萃取然后进行高效液相色谱-二极管阵列检测已被开发为一种同时,快速,准确,高效的样品制备方法,用于同时测定尿液样品中的七个有机紫外线滤光片。通过2〜((6-2))分数阶因子设计研究了主效应及其相互作用的影响。候选参数为:分散剂和萃取溶剂的类型和体积,样品的pH值和盐浓度。在最终最佳条件下,通过添加0.5 mL含70μL四氯化碳的乙腈(分散溶剂)(萃取溶剂)从5 mL样品中提取分析物,而无需改变溶液的pH值并应用(+1)盐浓度水平(10%w / v NaCl)。该测定是线性的(R〜2> 0.997),相对回收率在86.9%至97.3%之间,并且LOQ在3至45 ng mL〜(-1)之间。日内和日间RSD在线性范围的中点分别低于5和8%。所提出的方法已成功地应用于不同的志愿者尿液样品,并且表明提取效率不受尿液样品类型的影响。

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