利用無溶劑萃取技術快速測定環境固態樣品中之多環類麝香化合物的研究; Fast Determination of Synthetic Polycyclic Musks in Solid Samples by Solvent Free Techniques

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题名:	利用無溶劑萃取技術快速測定環境固態樣品中之多環類麝香化合物的研究;Fast Determination of Synthetic Polycyclic Musks in Solid Samples by Solvent Free Techniques
作者:	吳欣芳;Shin-Fang Wu
贡献者:	化學研究所
关键词:	氣相層析質譜儀;多環類麝香;固相微萃取法;Polycyclic Musks;GC-MS;SPME
日期:	2010-06-23
上传时间:	2010-12-08 14:16:33 (UTC+8)
出版者:	國立中央大學
摘要:	從古代開始，香氛就經常被用來增加對於個人的吸引力，而麝香因為在香精工業中被大量使用而佔有一席之地。多環類合成麝香作為天然麝香的平價替代品，在生產製造過程以及一般大眾使用後會隨著污水處理廠處理過後的污水及污泥排放到環境當中，而主要的污染源頭即為這些廢污水以及污泥。本篇研究中，利用一步完成的微波輔助頂空固相微萃取裝置搭配氣相層析質譜儀分析廢污泥、沉積物以及牡蠣樣品，方法不僅快速且不須使用有機溶劑。將除水後的固態樣品與20毫升的去離子水混合，以PDMS-DVB的塗附纖維置於樣品頂空後，使用80瓦微波，萃取5分鐘。此方法的偵測極限為0.04至0.1 ng/g，而定量極限為0.1至0.3 ng/g。對於這些環境樣品的初步檢測結果顯示，HHCB以及AHTN為最普遍被檢測到的兩種多環類麝香化合物，利用標準添加法進行定量分析，待測物的總濃度介於0.3至10.9 ng/g，而再現性的相對標準偏差範圍為4 %至10 %。本實驗所開發的微波輔助頂空固相微萃取法，搭配氣相層析質譜儀的選擇離子掃描偵測模式，為一種具有可靠性且靈敏度高的檢測方法，提供了一個方便的檢測技術以檢測環境固態樣品中微量的多環類麝香化合物。 Fragrances have been used increase attractiveness of persons since ancienttimes. Musk is one of the most important and often used fragrances in perfumery. Synthetic polycyclic musks are inexpensive substitutes for natural musks. Synthetic polycyclic musk compounds enter environment principally through effluents of wastewater treatment plants and waste sludge, and the major source of environmental pollution of synthetic musks is from sewage. In this study, one-step in situ microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis is presented as a fast and solvent-free technique to determine synthetic polycyclic musks in sewage sludge, sediment and oyster samples. The dewatered solid sample mixed with 20-mL deionized water was efficiently extracted by a polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber placed in the headspace when the extraction slurry was microwave irradiated at 80 W for 5 min. The limits of detection (LODs) ranged from 0.04 to 0.1 ng/g, and the limits of quantification (LOQs) ranged from 0.1 to 0.3 ng/g (fresh weight). A preliminary analysis of those samples revealed that HHCB and AHTN were the two most commonly detected synthetic polycyclic musks; using a standard addition method, their total concentrations were determined to rangefrom 0.3 to 10.9 ng/g (fresh weight) with relative standard deviation (RSD)ranging from 4% to 10%. The analytical procedure developed demonstrated that the MA-HS-SPME and GC-MS-SIM methods are reliable, sensitive and offer a convenient analytical technique for trace determination of polycyclic musks in various solid samples in environment.
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