Key Laboratory of Combinatorial Biosynthesis and Drug Discovery (Ministry of Education), and School of Pharmaceutical Sciences, Wuhan University, Wuhan, 430071, China.
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery (Ministry of Education), and School of Pharmaceutical Sciences, Wuhan University, Wuhan, 430071, China.
J Chromatogr A. 2019 Apr 26;1591:33-43. doi: 10.1016/j.chroma.2019.01.030. Epub 2019 Jan 11.
A novel supramolecular solvent (SUPRAS) based on hexafluoroisopropanol (HFIP)/Brij-35 was proposed for liquid-phase microextraction (LPME) of parabens in water samples, pharmaceuticals and personal care products. Brij-35 is a cost-effective and non-toxic non-ionic surfactant, but it has a high cloud point (>100 °C). HFIP, with the features of strong hydrogen-bond donor, high density and powerful hydrophobicity, was used as the cloud point-reducing agent and self-assembling and density-regulating solvent of Brij-35. Upon adding HFIP into the Brij-35 aqueous solution, the cloud point of Brij-35 was decreased to below room temperature, and the SUPRAS was formed in the bottom over a wide range of HFIP and Brij-35 concentrations at room temperature. The SUPRAS was composed of Brij-35, HFIP and water, having a density larger than water, and it showed a large spherical structure of positive micellar aggregates (2-8 μm). The HFIP/ Brij-35 SUPRAS-based LPME procedure was non-thermodependent and could be performed at room temperature with centrifugation using normal centrifuge tubes, being very simple. In the extraction of six parabens, the HFIP/ Brij-35 SUPRAS-based LPME method showed short extraction time (3.3 min), low solvent consumption (0.3 mL), and large enrichment factor (26-193). The method of HFIP/ Brij-35 SUPRAS-based LPME with HPLC-DAD gave good linearity for the quantification of parabens with correlation coefficients larger than 0.9990. The limits of detection based on a signal-to-noise ratio of 3 were from 0.042 to 0.167 μg L. The recoveries for the spiked real samples were in the range of 90.2-112.4% with relative standard deviation less than 8.9%. Except for tap water, one or several paraben (s) were detected in all the other real samples.
一种基于六氟异丙醇(HFIP)/Brij-35 的新型超分子溶剂(SUPRAS)被提出用于水样、药物和个人护理产品中对羟基苯甲酸酯的液相微萃取(LPME)。Brij-35 是一种经济有效且无毒的非离子表面活性剂,但它的浊点较高(>100°C)。HFIP 具有氢键供体强、密度高、疏水性强的特点,被用作降低 Brij-35 浊点的试剂和自组装及密度调节溶剂。当向 Brij-35 水溶液中加入 HFIP 时,Brij-35 的浊点降至室温以下,在室温下,HFIP 和 Brij-35 浓度较宽的范围内,在底部形成 SUPRAS。SUPRAS 由 Brij-35、HFIP 和水组成,密度大于水,呈现出大的正胶束聚集体的球形结构(2-8μm)。HFIP/ Brij-35 SUPRAS 基 LPME 过程是非热依赖性的,可以在室温下使用普通离心机管通过离心进行,非常简单。在六种对羟基苯甲酸酯的萃取中,HFIP/ Brij-35 SUPRAS 基 LPME 方法具有较短的萃取时间(3.3 分钟)、低溶剂消耗(0.3mL)和较大的富集因子(26-193)。HFIP/ Brij-35 SUPRAS 基 LPME 与 HPLC-DAD 联用的方法对 6 种对羟基苯甲酸酯的定量分析具有良好的线性关系,相关系数大于 0.9990。基于信噪比 3 的检测限为 0.042-0.167μg/L。实际样品的加标回收率在 90.2-112.4%之间,相对标准偏差小于 8.9%。除自来水外,所有其他实际样品中均检测到一种或几种对羟基苯甲酸酯(s)。