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1.
論文 |
鳥羽, 陽 ; 笠原, 千栄子 ; 戸次, 加奈江 ; 佐溝, 将之 ; 唐, 寧 ; 早川, 和一 ; Toriba, Akira ; Kasahara, Chieko ; Bekki, Kanae ; Samizo, Masayuki ; Ning, Tang ; Hayakawa, Kazuichi
概要:
金沢大学理工研究域自然システム学系<br />大気中の粒子状物質(PM)中の水酸化多環芳香族炭化水素(OHPAH)を定量することを目的とするGC/MSによる分析法を開発した.母核の環数が2〜4環のOHPAH 10種を分析対象とし,トリメチル
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シリル(TMS)誘導体化したうえで検出し,3種類の重水素化,または安定同位体標識化OHPAHを内部標準物質として用いてPM試料の定量に適用した.OHPAHのTMS誘導体の選択イオン検出(SIM)における検出限界(S/N=3)は,12〜930 fgの範囲で,すべての分析対象物質について10.5分で分離・検出することができた.都市大気標準粉じんや金沢で捕集したPM試料はジクロロメタンで抽出したのち,シリカゲル固相により精製しTMS誘導体化して定量した.金沢で捕集したPM試料中の8種のOHPAHを定量することに成功し,それらの濃度範囲は,20〜4100 fg m−3であり,3-hydroxyfluorantheneのPM中濃度の報告は本研究が初めてである.確立した分析法は,大気粉じん中のOHPAHを定量する際の分析法の選択肢の一つとして有用である.<br />A GC/MS method was developed for the quantification of hydroxylated polycyclic aromatic hydrocarbons (OHPAHs) in airborne particulate matter (PM). Ten OHPAHs having 2 - 4 rings were detected after trimethylsilyl (TMS) derivatization, and the derivatives in PM samples were quantified with three kinds of deuterated or stable isotope labeled OHPAHs as internal standards. The detection limits (S/N = 3) of the derivatives of OHPAHs in the selected ion monitoring (SIM) mode ranged from 12 to 930 fg and all analytes were separated and detected within 10.5 min. A commercially available urban PM sample and PM samples collected in Kanazawa were extracted with dichloromethane, and then the extracts were purified with silica gel solid phase and derivatized OHPAHs in the extracts were quantified. We successfully quantified 8 OHPAHs in PM samples collected in Kanazawa, and their concentrations were in the range of 20 - 4100 fg m−3 and the levels of 3-hydroxyfluoranthene were reported for the first time. This method should be useful as an optional analytical method to quantify OHPAHs in PM samples.
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2.
論文 |
鳥羽, 陽 ; 本間, 千春 ; 宇於崎, 和香 ; Chuesaard, Thanyarat ; 唐, 寧 ; 早川, 和一
概要:
A high-performance liquid chromatographic (HPLC) method with fluorescence detection was developed for the quantification
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of polycyclic aromatic hydrocarbons (PAHs) in cigarette mainstream and sidestream smoke particulates. Fifteen kinds of PAHs classified as priority pollutants by the US EPA were quantified with six perdeuterated PAHs as internal standards. The smoke filter samples obtained from 3 brands of cigarettes using standardized smoking conditions were extracted with dichloromethane, and then treated with tandem solid phase extraction cartridges (Silica and Neutral Alumina). The limits of detection ranged from 0.24 to 2.2 pg, and were more sensitive than those by GC-MS. The analytes were quantified by using the internal standards, and the developed method achieved sufficient reproducibility and accuracy. The PAH levels in mainstream and sidestream smoke from 3 cigarette brands were in the range of 0.2 – 305 ng cigarette−1 and 26.4 – 6160 ng cigarette−1, respectively. The total PAH content in sidestream smoke was more than 10 times higher compared with that of mainstream smoke. This method should be useful as an optional analytical method to quantify PAHs in cigarette smoke particulates.
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