摘要 本研究是針對四個二苯乙烯C.I.28、C.I.205、C.I.134和DAS1及一個二苯乙烯聯苯的DSBP螢光增白劑(Fluorescent Whitening Agents, FWAs)，發展出一套穩定、可靠的微量檢測技術，以測定這些物質在不同基質－洗衣用清潔劑、紙類、嬰幼兒衣物及環境中水樣中之含量。這個方法包括了在樣品前處理中－洗衣用清潔劑是以溶解、振盪及過濾三步驟完成;紙類和嬰幼兒衣物以hot-water extraction/SPE進行;水樣則是採用碳-18固相萃取法，以達到同時分離、萃取及去除干擾物質的目的，並藉由離子配對-高效液相層析儀搭配螢光偵測器(Ion-Pair HPLC/FLD)來加以定性及定量。 HPLC以C18當作層析管柱，藉由等速流析離子配對液相層析法可達到良好的分離，線性範圍為0.5 ~ 5?103 ng/L，線性相關係數0.999以上，定量偵測極限為0.1~0.01 µg/L。 本研究針對市面上常見之19種洗衣用清潔劑進行分析，結果顯示DSBP和DAS1是比較普遍使用添加於洗衣清潔劑中的FWAs。而hot-water extractiont成功地應用於紙類及嬰幼兒服飾的處理，利用碳-18萃取回收率分別為76~91%及81~92%，相對標準偏差分別在2.0~3.8%及3.1~4.0%之間。環境水樣實驗結果顯示，在添加FWAs於不同水樣時，其碳-18萃取回收率為72.6~89.4%，相對標準偏差在2.4~8.9%之間，而各個測點所偵測到的FWAs其相對標準也皆在3.0~5.8%之內，此說明了本套分析技術的穩定性及對複雜環境樣品中微量污染物檢測之可行性。 Abstract The purpose of this study is to develop a method for the analysis of four stilbene-type disulfonate and one distyrylbiphenyl-type fluorescent whitening agents (FWAs) in different matrixes: laundry detergents, papers and infant clothes, as well as river waters. The sample pretreatment methods involve: the laundry detergent using dissolved, filter and oscillation; the paper and infant cloth samples using a hot-water extraction with SPE; the water sample using the C18 SPE cartridge. The contents of FWAs were then determined by an isocratic ion-pair chromatography with C18 reversed- phase column, applying TBA as the ion-pair reagent, and equipped with fluorescent detection. No further sample cleanup procedures were necessary due to the sensitive and selective fluorescence detection. The accuracy and precision of the method was validated and was successfully applied to determine the contents of FWAs in laundry detergents, papers, infant clothes and surface waters. The quantitation limits were 0.1 to 0.01 ?g/L. The linear response was performed in the concentration covering the range from 0.05 to 500 ng/mL for DSBP, and 0.5 to 5000 ng/mL (in five-level) for other four FWAs. The calibration curve was linear with coefficients of determination r2 > 0.999. The precisions of the curves as indicated by R.S.D. of calibration factors (CF = peak area/amount) were 4.5 ~ 8.7%. For laundry detergents, the results show that the DSBP (0.5 to 2700 ?g/g) and DAS1 (29 to 980 ?g/g) are the two most added FWAs in detergents. For paper and infant cloth, recovery of FWAs in spiked paper and infant cloth samples was between 76 to 92% and precision (RSD) ranging from 2.0 to 4.0%. Analysis of six paper materials and three infant clothes found concentrations of FWAs ranging between 0.01 to 3.8 ?g/g and n.d. to 24 ?g/g, respectively. For river water, recovery of FWAs in spiked water samples was between 73 to 89% and precision (RSD) ranging from 2.4 to 8.9%. Analysis of for water samples found concentrations of FWAs ranging between 0.02 to 3.5 ?g/L. The results demonstrated that the developed method is reliable, and offering a convenient analytical technique for trace-level determination of FWAs in complex environmental samples.
