Wang Huazi, Hu Lu, Liu Xinya, Yin Shujun, Lu Runhua, Zhang Sanbing, Zhou Wenfeng, Gao Haixiang
Department of Applied Chemistry, College of Science, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Department of Applied Chemistry, College of Science, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
J Chromatogr A. 2017 Sep 22;1516:1-8. doi: 10.1016/j.chroma.2017.07.073. Epub 2017 Jul 22.
In the present study, a simple and rapid sample preparation method designated ultrasound-assisted dispersive liquid-liquid microextraction based on a deep eutectic solvent (DES) followed by high-performance liquid chromatography with ultraviolet (UV) detection (HPLC-UVD) was developed for the extraction and determination of UV filters from water samples. The model analytes were 2,4-dihydroxybenzophenone (BP-1), benzophenone (BP) and 2-hydroxy-4-methoxybenzophenone (BP-3). The hydrophobic DES was prepared by mixing trioctylmethylammonium chloride (TAC) and decanoic acid (DecA). Various influencing factors (selection of the extractant, amount of DES, ultrasound duration, salt addition, sample volume, sample pH, centrifuge rate and duration) on UV filter recovery were systematically investigated. Under optimal conditions, the proposed method provided good recoveries in the range of 90.2-103.5% and relative standard deviations (inter-day and intra-day precision, n=5) below 5.9%. The enrichment factors for the analytes ranged from 67 to 76. The limits of detection varied from 0.15 to 0.30ngmL, depending on the analytes. The linearities were between 0.5 and 500ngmL for BP-1 and BP and between 1 and 500ngmL for BP-3, with coefficients of determination greater than 0.99. Finally, the proposed method was applied to the determination of UV filters in swimming pool and river water samples, and acceptable relative recoveries ranging from 82.1 to 106.5% were obtained.
在本研究中，开发了一种基于深共熔溶剂（DES）的简单快速样品制备方法，即超声辅助分散液液微萃取，随后采用高效液相色谱-紫外检测（HPLC-UVD）法从水样中萃取和测定紫外线过滤剂。模型分析物为2,4-二羟基二苯甲酮（BP-1）、二苯甲酮（BP）和2-羟基-4-甲氧基二苯甲酮（BP-3）。通过混合氯化三辛基甲基铵（TAC）和癸酸（DecA）制备疏水性DES。系统研究了各种影响因素（萃取剂的选择、DES用量、超声时间、加盐量、样品体积、样品pH值、离心速率和时间）对紫外线过滤剂回收率的影响。在最佳条件下，该方法的回收率良好，在90.2%至103.5%之间，相对标准偏差（日间和日内精密度，n = 5）低于5.9%。分析物的富集因子在67至76之间。检测限因分析物而异，在0.15至0.30 ng/mL之间。BP-1和BP的线性范围为0.5至500 ng/mL，BP-3的线性范围为1至500 ng/mL，测定系数大于0.99。最后，将该方法应用于游泳池水和河水样品中紫外线过滤剂的测定，获得了82.1%至106.5%的可接受相对回收率。
