Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16815
標題: 液相層析質譜術於食用油中有機砷之研究
Determination of Organoarsenic Compounds in Edible Oil by Liquid Chromatography-Mass Spectrometry
作者: 王瑋珣
Wang, Wei-Hsun
關鍵字: Organoarsenic
有機砷
Liquid Chromatography-Mass Spectrometry
edible oil
arsenic
液相層析質譜
食用油
出版社: 化學系所
引用: [1] 楊志良, 行政院衛生署, 藥物食品安全週報第214期 2009年10月22日。 [2] 葉金川, 行政院衛生署, 藥物食品安全週報,第200期 2009年7月16日。 [3] 行政院衛生署,食用油脂中重金屬檢驗方法,九十六年七月十八日行政院衛生署署授食字第0961800223 號, 2007。 [4] M. J. Ruiz-Chanchoa, J. F. Lopez-Sancheza, E. Schmeisser, W. Goessler, K. A. Francesconi, R. Rubio, “Arsenic speciation in plants growing in arsenic-contaminated sites”, Chemosphere 71 (2008) 1522 [5] Z. Slejkovec, J. T. van Elteren, A. R. Byrne, J. J. M. de Goeij, “Separation of radiolabelled arsenic compounds produced by neutron irradiation of organoarsenic compounds” Analytica Chimica Acta 380 (1999) 63 [6] C. M. Liao, B. C. Chen, S. Singh, M. C. Lin, C. W. Liu, B. C. Han, “Acute Toxicity and Bioaccumulation of Arsenic in Tilapia”, Environmental Toxic ology 18 (2003) 252 [7] V. Nischwitz, S. A. Pergantis, “Improved Arsenic Speciation Analysis for Extracts of Commercially Available Edible Marine Algae Using HPLC-ES-MS/MS”, Journal of Agriculture Food Chemistry 54 (2006) 6507 [8] T. Kaise, S. Fukui, “The chemical form and acute toxicity of arsenic compounds in marine organisms”, Applied Organometallic Chemistry 6 (2004)155 [9] V. M. Dembitsky, Tomas Rezank, “Nature occurrence of arseno compounds in plants, lichens. Fungi. Algal species, and microorganisms”, Plant Science 165 (2003)1177 [10] “Environmental health criteria 18-arsenic”, World Health Organization Geneva 1981 [11] B. Szostek, J. H. Aldstadt, “Determination of organoarsenicals in the environment by solid phase Microextraction-gas chromatography-mass spectrometry”, Journal of Chromatography A 807 (2009)253 [12] 吳文菁,探討砷在關渡平原中水田與旱田土壤之分布,國立中興大學土壤環境科學系碩士學位論文,民國九十七年。 [13] A. H. Smith, E. O. Lingas, M. Rahman, “Contamination of drinking-water by arsenic in Bangladesh: a public health emergency”, Bulletin of the World Health Organization 78 (2000)1096. [14] J. W. Yager, J. K. Wiencke, “Enhancement of Chromosomal Damage by Arsenic: Implications for Mechanism”, Environnwntal Health Perspectives Supplements 101 (Suppl. 3) (1993)79. [15] 行政院衛生署,包裝飲用水及盛裝飲用水衛生標準,八十七年五月二日行政院衛生署衛署食87031964號,1998。 [16] V. K. Sharma, M. Sohn, “Aquatic arsenic: Toxicity, speciation, transformations, and remediation” , Environment International 35 (2009) 743 [17] A. J. Bednar, J. R. Garbarino, J. F. Ranville, T. R. Wildeman, “Presence of Organoarsenicals Used in Cotton productiob in Agricultural Water and Soil of the Southern United States”, Journal of Agriculture Food Chemistry 50 (2002) 7340. [18] Z. Gong, X. Lu, M. Ma, C. Watt, X. C. Le, “Arsenic speciation analysis”, Talanta 58 (2002) 77 [19] C. Tu, L. Q. Ma, W. Zhang, Y. Cai, W. G. Harris, “Arsenic species and leachability in the fronds of the hyperaccumulator Chinese brake (Pteris vittata L.)”, Environmental Pollution 124 (2003) 223 [20] C. Yuana, E. Gaoa, B. Hea, G. Jiang, “Arsenic species and leaching characters in tea (Camellia sinensis)”, Food and Chemical Toxicology 45 (2007) 2381 [21] F.R. Gilbert, G.A.H. Wells, R.F. Guning, “3-nitro-4 -hydroxyphenylarsonic acid toxicity in pigs.”, Veterinary Record 109 (1981)158. [22] A. C. Schmidt, K. Kutschera, J. Mattusch, M. Otto, “Analysis of accumulation, extractability, and metabolization of five different phenylarsenic compounds in plants by ion chromatography with mass spectrometric detection and by atomic emission spectroscopy”, Chemosphere 73 (2008) 1781 [23] P. Wang, G. Zhao, J. Tian, X. Su, “High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry Based Method for the Determination of Organic Arsenic Feed Additives and Speciation of Anionic Arsenics in Animal Feed”, Journal of Agriculture Food Chemistry, 50 (2010) 5263. [24] V. Nischwitz, S. A. Pergantis, “Liquid Chromatography Online with Selected Reaction Monitoring Electrospray Mass Spectrometry for the Determination of Organoarsenic Species in Crude Extracts of Marine Reference Materials”, Analytical Chemistry 77(2005) 5551 [25] M. V. Hulle, C. Zhang, X. Zhang, R. Cornelis, “Arsenic speciation in Chinese seaweeds using HPLC-ICP-MS and HPLC-ES-MS”, Analyst 127 (2002) 634 [26] R. Schaeffer, P. Fodor, C. Soeroes, “Development of a liquid chromatography/electrospray selected reaction monitoring method for the determination of organoarsenic species in marine and freshwater samples”, Rapid Communication in Mass Spectrometry 20 (2006) 2979. [27] 唐永安,以HPLCUV同步分析砷物種之研究,國立中興大學化學系碩士學位論文,民國八十三年 [28] Y.T. Chang, S. J. Jiang, “Determination of As, Cd and Hg in emulsified vegetable oil by flow injection chemical vapour generation inductively coupled plasma mass spectrometry”, Journal of Analytical Atomic Spectrometry 23(2008)140 [29] X. H. Zang, Q. H.Wu, M. Y. Zhang, G. H. Xi, Z. Wang, “Developments of Dispersive Liquid-Liquid Microextraction Technique”, Chinese Journal of Analytical Chemistry 37 (2009)161. [30] M. Rezaee, Y. Yamini, M. Faraji, “Evolution of dispersive liquid–liquid microextraction method”, Journal of Chromatography A 1217 (2010) 2342 [31] M. B. Melwanki, M. R. Fuh, ”Partitioned dispersive liquid–liquid Microextraction An approach for polar organic compounds extraction from aqueous samples”, Journal of Chromatography A 1207 (2008) 24 [32] M. Rezaee, Y. Assadi, M. R. M. Hosseini, E. Aghaee, F. Ahmadi, S. Berijani, “Determination of organic compounds in water using dispersive liquid–liquid microextraction”, Journal of Chromatography A 1116 (2006) 1 [33] S. Berijani, Y. Assadi, M. Anbia, M. R. M. Hosseini, E. Aghaee, “Dispersive liquid–liquid microextraction combined with gas chromatography-flame photometric detection Very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water”, Journal of Chromatography A 1123 (2006) 1 [34] M. D. L. de Castro, F. Priego-Capote, “Ultrasound-assisted preparation of liquid samples”, Talanta 72 (2007) 321 [35] S.L. Lin, M. R. Fuh, “Orthogonal array optimization of ultrasound-assisted emulsification–microextraction for the determination of chlorinated phenoxyacetic acids in river water”, Journal of Chromatography A 1217 (2010) 3467 [36] 周繼琪,質譜術於藥物及其代謝物和環境汙染物之分析,國立中興大學化學系博士學位論文,民國九十四年。 [37] 姚佳君,液相層析質譜術於動物組織中硝砆喃代謝物之偵測,國立中興大學化學系碩士學位論文,民國九十八年。 [38] C. Dass, “Fundamentals of contemporary mass spectrometry, Chepter 2”, John Wiley&Sons (2007) [39] J. Gilman, C. Mashburn, “Electrospray Ionization Mass spectrometry” 2002 Chemistry 5181. [40] P. Gates, “Mass spectrometer source”, The University of Bristol, School of Chemistry, 2004. [41] 李茂榮,科儀叢書5質譜分析專輯 第五章,行政院國家科學委員會精密儀器發展中心編印. [42] 陳崇宇,質譜術於尿液中ketamine及其新陳代謝體偵測之研究,國立中興大學化學系碩士學位論文,民國九十一年。 [43] 陸冠輝,固相微萃取結合液相層析質譜儀於磺胺類劑之偵測,國立中興大學化學系碩士學位論文,民國九十二年。 [44] Finnigan LCQ, MS Detector Hardware Manual. [45] 洪晟翰,吹氣輔助頂空固相微萃取結合氣相層析質譜術於水中多環芳香烴之研究,國立中興大學化學系碩士學位論文,民國九十七年。 [46] F.Y. Du, X. H. Xiao, G. K. Li, “Application of ionic liquids in the microwave-assisted extraction of trans-resveratrol from Rhizma Polygoni Cuspidati”, Journal of Chromatography A 1140 (2007) 56 [47] M. B. Melwanki, M. R. Fuh, “Dispersive liquid–liquid microextraction combined with semi-automated in-syringe back extraction as a new approach for the sample preparation of ionizable organic compounds prior to liquid chromatography”, Journal of Chromatography A 1198–1199 (2008) 1 [48] P. Hashemi, S. Beyranvand, R. S. Mansur, A. R. Ghiasvand, “Development of a simple device for dispersive liquid–liquid microextraction with lighter than water organic solvents: Isolation and enrichment of glycyrrhizic acid from licorice”, Analytica Chimica Acta 655 (2009) 60 [49] E. Z. Jahromi, A. Bidari, Y. Assadi, M. R. M. Hosseini, M. R. Jamali, ” Dispersive liquid–liquid microextraction combined with graphite furnace atomic absorption spectrometry Ultra trace determination of cadmium in water samples”, Analytical Chimical Acta 585 (2007) 305
摘要: 本實驗試探討以超音波輔助分散液液微結合液相層析質譜術進行分析應用於食用油中三種有機砷monomethylarsenic acid (MMA), dimethylarsenic acid (DMA) 和 3-nitro-4-hydroxyphenylarsonic acid (Roxarsone)之研究。本實驗探討分散溶劑種類、萃取溶劑pH值、萃取時間及分散溶劑和萃取溶劑的體積等對萃取效率之影響,並利用正交設計表求出實驗條件的最佳化。 實驗結果顯示以超音波輔助分散液液微萃取結合液相層析質譜術於電灑游離法正離子模式分析,使用1.2 mL正己烷為分散溶劑、 pH 7的甲酸銨緩衝溶液50μL為萃取溶劑,萃取時間為4分鐘時能得到最好的萃取效率。將此技術應用於食用油分析,偵測線性範圍MMA為25~500 ng/g,DMA為5~500 ng/g,Roxarsone為10~500 ng/g,線性相關係數在0.9946以上,偵測極限在1~5.8 ng/g之間。其回收率為78.2%~107.3%,相對標準偏差在2.2%~11.0%之間。intra-day精密度為1.6% ~13.8%,inter-day為7.9% ~18.2%。將此技術應用於真實樣品中分析,在回鍋油中測得含DMA濃度為6.0 ng/g,證明此方法可成功的應用在食用油中有機砷的分析。
In this study, a simple, efficient and rapid method of ultrasound-assisted dispersive liquid liquid microextraction (UADLLME) has been developed for extraction and preconcentration of three organoarsenic compounds, monomethylarsenic acid (MMA), dimethylarsenic acid (DMA) and 3-nitro-4-hydroxyphenylarsonic acid (Roxarsone) in edible oil. The extraction was analyzed by using liquid chromatography-mass spectrometry. The parameters affected on the extraction efficiency such as the type of dispersive solvent, the pH value of extraction solvent, the extraction time, volume of dispersive solvent and extraction solvent were using Orthogonal array design to be examined and optimized. From the results, the optimum conditions were 1.2 mL hexane used as dispersive solvent, 50μL of pH 7 buffer solution as extraction solvent for extraction 4 minutes. Under the optimum conditions, the recoveries of organoarsenic compounds in edible oil at 25 ng/g, 100 ng/g and 500 ng/g were ranging from 78.2% to 107.3%. The relative standard deviations varied from 2.2% to 11.0% (n=3). The linearity of the method was from 25 to 500 ng/g for MMA, 5 to 500 ng/g for DMA and 10 to 500 ng/g for Roxarsone. The correlation coefficients were from 0.9946 to 0.999. The LOD was from 1 ng/g to 5.8ng/g and the LOQ was from 3.3 ng/g to 19.2 ng/g. The precisions (RSD%) were obtained in the range from 1.6% to 13.8% for intra-day (n=5) and 7.9% to 18.2% for inter-day (n=5). The ultrasound-assisted dispersive liquid liquid microextraction combined with LC-MS was successfully applied to the analysis of trace organoarsenic compounds in edible oil.
URI: http://hdl.handle.net/11455/16815
其他識別: U0005-2307201007145600
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