Canosa P, Rodríguez I, Rubí E, Cela R
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y AnAlisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
Anal Chem. 2007 Feb 15;79(4):1675-81. doi: 10.1021/ac061896e.
A simple sample preparation method for the determination of four parabens and triclosan in indoor dust is presented. Analytes were extracted from the sample and isolated from interfering species using the matrix solid-phase dispersion technique. After that, they were silylated and determined by gas chromatography combined to tandem mass spectrometry (GC/MS/MS). The influence of several factors on the yield and selectivity of the extraction was evaluated in detail. Under final working conditions, samples (0.5 g) were mixed with the same amount of anhydrous sodium sulfate and dispersed on 1.25 g of C18. This blend was transferred to the top of a polypropylene cartridge containing 2 g of Florisil. After removing less polar species with 10 mL of dichloromethane, analytes were recovered using 10 mL of acetonitrile. This extract was concentrated to 1 mL, derivatized, and injected in the GC/MS/MS system. Derivatization was carried out at 45 degrees C in 5 min using 100 microL of N-methyl-N-(tert-butyldimethylsilyl) trifluoroacetamide. Quantification limits from 0.6 to 2.6 ng/g and absolute recoveries between 80 and 114% were achieved. Analysis of dust samples demonstrated the presence of the target species in indoor dust from private houses. The highest average concentration (702 ng/g) corresponded to triclosan.
本文介绍了一种用于测定室内灰尘中四种对羟基苯甲酸酯和三氯生的简单样品制备方法。使用基质固相分散技术从样品中提取分析物,并将其与干扰物质分离。之后,对其进行硅烷化处理,并用气相色谱-串联质谱联用仪(GC/MS/MS)进行测定。详细评估了几个因素对萃取产率和选择性的影响。在最终工作条件下,将样品(0.5 g)与等量的无水硫酸钠混合,并分散在1.25 g的C18上。将此混合物转移至装有2 g弗罗里硅土的聚丙烯柱顶部。用10 mL二氯甲烷去除极性较小的物质后,用10 mL乙腈回收分析物。将此提取物浓缩至1 mL,进行衍生化处理,然后注入GC/MS/MS系统。使用100 μL N-甲基-N-(叔丁基二甲基硅烷基)三氟乙酰胺在45℃下5分钟内进行衍生化。实现了0.6至2.6 ng/g的定量限和80%至114%的绝对回收率。灰尘样品分析表明,私人住宅室内灰尘中存在目标物质。最高平均浓度(702 ng/g)对应于三氯生。