摘要
本文建立了纤维制品中游离甲醛的固相萃取-气质联用测定方法。试样剪碎后置于饱和NaCl溶液中60℃超声处理30min,经五氟苯盐酸羟胺(PFBOA)衍生化后,采用顶空固相微萃取和色质联用技术(HS-SPME—GC/MS),选择离子(m/z181)进行定量。该方法适用于各类单层或多层纤维织物中甲醛的测定,加标回收率分别为94.9%~98.7%,相对标准偏差(RSD)在2.97%~4.59%之间,检出限为0.02mg/kg。
A method has been developed for determination of formaldehyde in fibre products by GC-MS using headspace solid phase extraction. Samples were treated with 1 mg/mL o-(2, 3, 4, 5, 6- Pentafluorobenzyl) hydroxylamine (PFBOA) in a sealed vial at 60℃ for 30 min. Headspace solid-phase microextraction (SPME) was then performed with 65 μm PDMS/DVB, and the extracts were directly analyzed by gas chromatography/mass spectrometry (GC/MS) under selective ion method (SIM) mode. This headspace SPME GC/MS method was highly sensitive to the target compound because it eliminates interference from the sample matrix solution. The limits of detection were 0. 02 mg/kg with average recoveries between 94.9%-98.7% at the different spiking levels. The relative standard deviation (RSD) of the method for the spiked samples was 2. 97%- 4.59%.
出处
《分析科学学报》
CAS
CSCD
2006年第6期693-696,共4页
Journal of Analytical Science