Negreira N, Rodríguez I, Rubí E, Cela R
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
J Chromatogr A. 2009 Jul 31;1216(31):5895-902. doi: 10.1016/j.chroma.2009.06.020. Epub 2009 Jun 10.
A simple, inexpensive sample preparation procedure, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six UV filters: 2-ethylhexyl salicylate (EHS), 3,3,5-trimethylcyclohexyl salicylate (Homosalate, HMS), 3-(4-methylbenzylidene) camphor (4-MBC), isoamyl-p-methoxycinnamate (IAMC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene (OCR), in dust from indoor environments is presented and the influence of several operational parameters on the extraction performance discussed. Under the final working conditions, sieved samples (0.5 g) were mixed with the same amount of anhydrous sodium sulphate and dispersed with 2 g of octadecyl bonded silica (C18) in a mortar with a pestle. This blend was transferred to a polypropylene solid-phase extraction cartridge containing 2 g of activated silica, as the clean-up co-sorbent. The cartridge was first rinsed with 5 mL of n-hexane and the analytes were then recovered with 4 mL of acetonitrile. This extract was adjusted to 1 mL, filtered and the compounds were determined by gas chromatography combined with tandem mass spectrometry (GC-MS/MS). Recoveries for samples spiked at two different concentrations ranged between 77% and 99%, and the limits of quantification (LOQs) of the method between 10 and 40 ng g(-1). Analysis of settled dust from different indoor areas, including private flats, public buildings and vehicle cabins, showed that EHMC and OCR were ubiquitous in this matrix, with maximum concentrations of 15 and 41 microg g(-1), respectively. Both UV filters were also quantified in dust reference material SRM 2585 for first time. EHS, 4-MBC and IAMC were detected in some of the analyzed samples, although at lower concentrations than EHMC and OCR.
本文介绍了一种基于基质固相分散（MSPD）技术的简单、廉价的样品制备方法，用于测定室内环境灰尘中的六种紫外线过滤剂：2-乙基己基水杨酸酯（EHS）、3,3,5-三甲基环己基水杨酸酯（胡莫柳酯，HMS）、3-(4-甲基亚苄基)樟脑（4-MBC）、异戊基对甲氧基肉桂酸酯（IAMC）、2-乙基己基对甲氧基肉桂酸酯（EHMC）和奥克立林（OCR），并讨论了几个操作参数对萃取性能的影响。在最终工作条件下，将过筛后的样品（0.5 g）与等量的无水硫酸钠混合，并用2 g十八烷基键合硅胶（C18）在研钵中用杵研磨分散。将此混合物转移至装有2 g活化硅胶作为净化共吸附剂的聚丙烯固相萃取柱中。先用5 mL正己烷冲洗柱子，然后用4 mL乙腈回收分析物。将此提取物调至1 mL，过滤，并用气相色谱-串联质谱联用仪（GC-MS/MS）测定化合物。在两种不同浓度下加标的样品回收率在77%至99%之间，该方法的定量限在10至40 ng g⁻¹之间。对来自不同室内区域（包括私人公寓、公共建筑和车厢）的沉降灰尘进行分析表明，EHMC和OCR在该基质中普遍存在，最高浓度分别为15和41 μg g⁻¹。这两种紫外线过滤剂也首次在灰尘标准物质SRM 2585中被定量。在一些分析样品中检测到了EHS、4-MBC和IAMC，尽管其浓度低于EHMC和OCR。
