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Please use this identifier to cite or link to this item: http://ntour.ntou.edu.tw:8080/ir/handle/987654321/35024

Title: 食品中動物用藥殘留檢測方法開發及殘留監測
Development of Detection Method and Residue Monitoring of Veterinary Drugs in Foods
Authors: 唐玉芸
Contributors: NTOU:Department of Food Science
國立臺灣海洋大學:食品科學系
Keywords: 動物用藥;抗生素;多重殘留;液相層析串聯質譜儀
veterinary drugs;antibiotics;multi-residue;liquid chromatography tandem mass spectrometry
Date: 2012
Issue Date: 2013-10-07T02:49:37Z
Abstract: 以液相層析串聯質譜儀(liquid chromatography method with tandem mass, LC-MS/MS)利用三段四極棒式 (triple-quadrupole) 質譜儀,以電灑法離子化配合正、負離子偵測模式,檢測動物用藥殘留量之分析為主要方法開發及檢測工具,分別檢測食品中之不同動物用藥殘留分析,以符合現代化精密微量之檢驗技術,進而建立國內市售產品中之殘留量調查方法,期供政府及學術檢驗單位之參考。 本論文首先建立以液相層析串聯質譜法分析食品中殘留氯黴素之檢驗方法。移動相溶液以0.1 % 甲酸溶液及甲醇進行梯度分析,使用層析管柱為Hypersil C18,3 μm,內徑 2.1 x 50 mm,以電灑負離子模式選擇母離子m/z 321及主要子離子片段為m/z 152、257及194,以m/z 152為定量子離子,利用離子片段訊號之滯留時間、訊號面積及子離子間訊號強度比值作為定性及定量之依據。萃取液為乙酸乙酯,經由液-液相萃取淨化方式可得到良好之回收率與淨化效果,具有良好之再現性,於雞肉、魚肉、蝦肉及蜂蜜中平均回收率分別為90.1%、78.3%、76.2%與109.3%。 為檢測雞蛋及鮮乳中殘留5種離子攜帶型抗生素之多重檢測,以液相層析串聯質譜法分析。實驗步驟為取全蛋及鮮乳加入無水硫酸鈉,混合均勻直到呈現小顆粒球狀,經乙腈萃取後,經氮氣濃縮後,選用XTerraTM Phenyl之層析管柱,搭配0.1 % 甲酸水溶液與乙腈梯度變換比例進行層析。此方法之雞蛋及鮮乳平均回收率,分別為90.5~95.0%及95.0~104.7%,檢測限量為0.5~1.5 ppb間,並提供了快速、有效的檢驗方法,可減少人力及實驗耗費,增加檢驗的時效性。 為開發食品中抗生素多重殘留分析方法,乃使用液相層析串聯質譜儀分析食品基質中巨環類(macrolides)抗生素、β-內醯胺類(β-lactams)抗生素、林可黴素類(lincosamides) 抗生素及其他類抗生素。本研究開發了肌肉中殘留18種抗生素及牛奶中殘留23種抗生素之快速多重殘留分析方法。實驗步驟為肌肉檢體以0.2% 偏磷酸和甲醇混合溶液 (3 : 7, v/v)及磷酸鹽緩衝液 (phosphate buffer saline, PBS)萃取,選用Oasis HLB之固相萃取匣作為淨化程序;牛奶檢體以乙腈萃取,經氮氣濃縮後,選用ACQUITY UPLC HSS T3之層析管柱,搭配0.005 % 甲酸水溶液與乙腈進行質譜分析。禽畜肉類檢體添加18種抗生素後回收率除neospiramycin及mecillinam外,介於60~120%間,變異係數小於20%;魚肉檢體回收率除林可黴素及orbifloxacin外,介於60~120%間;牛奶檢體回收率介於60~120%間。本方法有減少人力及實驗耗費,增加檢驗時效性之優點。
A liquid chromatography method with tandem mass (LC-MS/MS) by using electrospray negative ion mode detection and identification is presented for the determination of chloramphenicol in foods. The analytes were extracted with ethylacetate and defatted with n-hexane by liquid-liquid extraction. The column was a Hypersil C18 (2.1 x 50 mm, 3 μm) with a mixture of 0.1% formic acid water and methanol by gradient mobile phase. The electrospray negative ionization produced the parent molecular ions at m/z 321 and produced three characteristic transition reaction fragments (m/z 321 →152, 257 and 194). The recovery rate of developed method was 90.1%, 78.3%, 76.2%, and 109.3% in chicken meat, fish meat, shrimp meat and honey, respectively. A sensitive and selective LC-MS/MS method for the simultaneous detection of five ionophore coccidiostats was developed. The method used a simple extraction technique with acetonitrile and a minimal sample purification procedure to decrease the time needed before MS system analysis. The analysis time on the MS system was about 15 min; and this method revealed lasalocid, maduramicin, and salinomycin contamination in eggs and maduramicin contamination in milk purchased in Taiwan. Therefore, this method provides not only qualitative analysis but quantification of residues in food and environmental contamination. A rapid multi-residue/multi-class procedure utilizing ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) detection has been developed and validated to monitor veterinary drugs. This article presents a method for the determination and confirmation of 18 veterinary drugs in muscle and 23 drugs in milk. The optimized procedure was then used to analyze commercial milk in Taiwan and proved to be a fast and simple method that can be applied in routine laboratory analysis of large numbers of samples containing different families of compounds.
URI: http://ethesys.lib.ntou.edu.tw/cdrfb3/record/#G0D92320006
http://ntour.ntou.edu.tw/handle/987654321/35024
Appears in Collections:[食品科學系] 博碩士論文

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