Benedé Juan L, Chisvert Alberto, Giokas Dimosthenis L, Salvador Amparo
Department of Analytical Chemistry, University of Valencia, 46100 Burjassot, Valencia, Spain.
Department of Analytical Chemistry, University of Valencia, 46100 Burjassot, Valencia, Spain.
Talanta. 2016 Jan 15;147:246-52. doi: 10.1016/j.talanta.2015.09.054. Epub 2015 Sep 26.
In this work, a new approach that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive solid phase extraction (DSPE), i.e. stir bar sorptive-dispersive microextraction (SBSDµE), is employed as enrichment and clean-up technique for the sensitive determination of eight lipophilic UV filters in water samples. The extraction is accomplished using a neodymium stir bar magnetically coated with oleic acid-coated cobalt ferrite magnetic nanoparticles (MNPs) as sorbent material, which are detached and dispersed into the solution at high stirring rate. When stirring is stopped, MNPs are magnetically retrieved onto the stir bar, which is subjected to thermal desorption (TD) to release the analytes into the gas chromatography-mass spectrometry (GC-MS) system. The SBSDµE approach allows for lower extraction time than SBSE and easier post-extraction treatment than DSPE, while TD allows for an effective and solvent-free injection of the entire quantity of desorbed analytes into GC-MS, and thus achieving a high sensitivity. The main parameters involved in TD, as well as the extraction time, were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ngL(-1) range and good intra- and inter-day repeatability (RSD<12%). This accurate and sensitive analytical method was applied to the determination of trace amounts of UV filters in three bathing water samples (river, sea and swimming pool) with satisfactory relative recovery values (80-116%).
在本研究中,一种结合了搅拌棒吸附萃取(SBSE)和分散固相萃取(DSPE)优点的新方法,即搅拌棒吸附-分散微萃取(SBSDµE),被用作富集和净化技术,用于灵敏测定水样中的8种亲脂性紫外线过滤剂。萃取过程使用涂有油酸包覆钴铁氧体磁性纳米颗粒(MNPs)的钕搅拌棒作为吸附材料,在高搅拌速率下,这些磁性纳米颗粒会脱离并分散到溶液中。停止搅拌时,磁性纳米颗粒会通过磁力吸附到搅拌棒上,然后对搅拌棒进行热解吸(TD),将分析物释放到气相色谱-质谱(GC-MS)系统中。SBSDµE方法比SBSE所需的萃取时间更短,且比DSPE的萃取后处理更简便,而热解吸能将全部解吸分析物有效且无溶剂地注入GC-MS,从而实现高灵敏度。对热解吸过程中涉及的主要参数以及萃取时间进行了评估。在优化条件下,该方法成功得到验证,具有良好的线性、低ngL(-1)范围内的检测限和定量限,以及良好的日内和日间重复性(RSD<12%)。这种准确且灵敏的分析方法被应用于测定三个沐浴水样(河流、海洋和游泳池)中的痕量紫外线过滤剂,获得了令人满意的相对回收率(80-116%)。