Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, Campus Sur. Universidad de Santiago de Compostela, E-15782, Santiago de Compostela, Spain.
Chemosphere. 2010 Dec;81(11):1378-85. doi: 10.1016/j.chemosphere.2010.09.028.
A method based on ultrasound-assisted emulsification-microextraction (USAEME) and gas chromatography-mass spectrometry (GC-MS) has been developed for the analysis of regulated fragrance allergens in water. Extraction conditions such as the type of solvent, extraction temperature, irradiation time, and salting-out effect were optimized using a multivariate approach. Compounds were extracted during 2 min in an acoustically emulsified media formed by 100 μL chloroform and 10 mL sample. The USAEME process provided an efficient and exhaustive extraction (enrichment factor ∼100) and, after centrifugation, the extract was ready for GC analysis. Validation was performed using spiked ultrapure water as well as other most complex matrices such as sewage water. Recoveries between 75% and 110% were generally obtained, and precision was characterized by RSD values <10% in most cases. The limits of detection (LODs) were at the sub-nanogram per millilitre level. The proposed procedure was applied to the determination of allergens in several real samples including tap water, baby bathwater, recreational place water, public washing place water, and sewage water. The presence of some of the target compounds was confirmed in all the samples excluding tap water, demonstrating the ubiquity of this group of cosmetic and personal care products ingredients.
一种基于超声辅助乳化-微萃取(USAEME)和气相色谱-质谱联用(GC-MS)的方法已被开发用于分析水中受规管的香料过敏原。通过多变量方法优化了溶剂类型、萃取温度、辐照时间和盐析效应等萃取条件。在 100 μL 氯仿和 10 mL 样品形成的声乳化介质中,化合物在 2 分钟内被提取。USAEME 过程提供了高效和彻底的提取(富集因子约为 100),离心后,萃取物即可用于 GC 分析。使用加标超纯水以及其他更复杂的基质(如污水)进行了验证。回收率一般在 75%至 110%之间,大多数情况下,精密度用 RSD 值<10%来表示。检出限(LOD)达到纳克每毫升以下的水平。该方法已应用于测定包括自来水、婴儿沐浴水、娱乐场所水、公共洗涤场所水和污水在内的几种实际样品中的过敏原。除自来水外,所有样品中均确认存在部分目标化合物,这表明此类化妆品和个人护理产品成分无处不在。