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  • 學位論文

微波輔助酸消化與離子層析法配合感應耦合電漿質譜儀於檳榔及荖葉中多重元素與砷物種分析之研究

Multielemental analysis and arsenic speciation in betel nut and piper leaf by microwave assisted digestion, ion chromatography and inductively coupled plasma-mass spectrometry

指導教授 : 黃友利
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摘要


嚼食檳榔會引發各種口腔疾病與相關癌症的發生,全世界檳榔嚼食人口相當多,在台灣目前約有200多萬的檳榔嚼食人口。近年來研究顯示嚼食檳榔與抽煙或飲酒為造成口腔病變的重要危險因子之一,然而檳榔中微量元素與微量金屬物種的分析,卻鮮有相關研究予以探討。因此,本研究利用微波輔助酸消化方法配合感應耦合電漿質譜法進行檳榔與荖葉中微量元素(鎵、砷、鉬、銀、鎘、錫、鉛)總量分析。此外,本研究也利用液相萃取法配合高效能液相層析-感應耦合電漿質譜儀連線系統進行檳榔與荖葉中砷物種之分析。在多元素總量分析方面,以硝酸:過氧化氫比例6:2與7:1為消化液,配合20與25分鐘之消化時間進行微波輔助酸消化,可分別有效消化檳榔與荖葉樣品。在砷物種分析方面,以75%(v/v)甲醇,萃取溫度80, 70℃與萃取時間15分鐘,可達到萃取出檳榔與荖葉中砷物種之目的。在多元素分析的分析效能方面,研究結果顯示各待測元素之檢量線之線性相關係數皆大於0.995、精密度(RSD,%)皆低於3.0%、大多數待測元素之標準添加回收率介於80-120%間;經利用標準參考樣品NIST SRM1567a分析驗證,顯示本方法的可行性;此方法對砷、銀、鎘、鎵、鉬、鉛、錫的偵測極限分別為0.016、0.040、0.003、0.020、0.040、0.010及0.170 µg/L。在砷物種分析方面,四種砷物種(arsenite, arsenate, monomethylarsonicacid, dimethylarsinic acid) 標準檢量線之線性相關係數皆大於0.995,精密度皆低於5.0% ,由於並無砷物種之標準參考物質可供使用,以標準添加回收率進行方法準確度之確認,結果顯示其回收率介於87.1-114.6%之間。將所開發之分析方法應用於真實樣品檢測上發現,本研究所分析之檳榔及荖葉中重金屬含量皆在法規限值之內,而在砷物種分析則顯示檳榔中四種砷物種濃度皆低於方法偵測極限,而荖葉中存在之砷物種則以無機砷物種為主。

並列摘要


Chewing betel quid will result in oral diseases and carcinoma. In Taiwan, where the practice of betel quid chewing is widespread, approximately two million people chew betel quid habitually. Recent studies have shown that betel quid chewing is an important risk factor for oral cancer similar to alcohol drinking and cigarette smoking. However, few studies have been devoted to the analysis of trace elements and metal species in betel nut and piper leaf. In the present study, a microwave-assisted digestion method with inductively coupled plasma mass spectrometry (ICP-MS) detection was developed for the simultaneous determination of arsenic (As), cadmium (Cd), cobalt (Co), molybdenum (Mo), silver (Ag), gallium (Ga) and lead (Pb) in the betel quid samples. In addition, we used HPLC coupled with ICP-MS for arsenic speciation in betel nut and piper leaf. Parameters such as acid/oxidizing reagents concentrations, acid/oxidizing solution volume, temperature, ramp time and hold time for the microwave-assisted digestion were investigated. Under the optimized conditions, the linearity, precision, accuracy and detection limit of the proposed methods were evaluated. The precision below 5.0 % RSD for the elements of interest was obtained. The accuracy evaluated with spike recovery and standard reference material (NIST SRM 1573a) was found to be acceptable. The limit of detection for As, Ag, Cd, Ga, Mo, Pb and Sn was 0.016, 0.040, 0.003, 0.020, 0.040, 0.010 and 0.170 µg/L, respectively. The analytical performance of the proposed method for arsenic speciation was evaluated and found to be reliable for the determination of arsenite, arsenate, monomethylarsonicacid, dimethylarsinic acid in betel nut and piper leaf. The levels of the seven elements of interest in this study were observed within the laws and regulations limiting value. Moreover, inorganic arsenic species was found to be the predominant arsenic species in piper leaf.

參考文獻


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