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標題: 液相層析質譜術於動物組織中硝基呋喃代謝物之偵測
Determination of nitrofuran metabolites in animal tissue by liquid chromatography-tandem mass spectrometry
作者: 姚佳君
Yao, Chia-Chun
關鍵字: liquid chromatography-tandem mass spectrometry
animal tissue
出版社: 化學系所
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摘要: 本實驗使用微波輔助衍生化法結合液相層析質譜,利用加熱式電灑游離法,以高解析選擇反應偵測模式為定量方式,進行動物組織中硝基呋喃代謝物偵測。本實驗偵測四種硝基呋喃代謝物包含Semicarbazide hydrochloride(SC)、3-amino-2-oxazolidinone(AOZ)、1-aminohydantoin hydrochloride(AH)、3-amino-5-morpholinomethyl- 2-oxazolidinone(AMOZ)。實驗探討微波功率、微波時間、衍生化試劑體積、萃取溶劑種類以及萃取溶劑體積對衍生化效果之影響,並以正交設計表找出實驗最佳化參數。並探討此技術之線性範圍、偵測極限、回收率及再現性。 實驗結果顯示當微波功率於250瓦,微波時間為7秒,衍生化試劑體積為300 μL,並以乙酸乙酯5 mL為萃取溶劑條件下,可得到最佳實驗結果。將此技術應用於真實肉類樣品,於加熱式電灑游離法以及高解析選擇反應偵測模式可得到線性範圍在0.3 ng/g-50 ng/g (SC為0.5ng/g-50ng/g)之間。偵測極限在2.9-11.7 pg/g之間,線性相關係數在0.995以上。將此方法應用於真實雞肉樣品可偵測到15.6 ng/g之SC含量,故本技術可做為動物組織樣品中硝基呋喃代謝物確認技術之依據。
The aim of this study is to develop a rapid microwave-assisted derivatization method combined with liquid chromatography-tandem mass spectrometry (LC-MS-MS) to determine of four nitrofuran metabolites in animal's tissue. The derivatization parameters including microwave power, microwave time, volume of derivatization reagent and extraction solvent were studied by using a uniform experimental design at four levels. The optimal conditions obtained were at irradiation of 250W microwave for 7s and ethyl acetate used as extraction reagent. The method was performed by the heated electrospray ionization (H-ESI) and highly-selective reaction monitoring (H-SRM) to obtain high ionization efficiency and reduce the interference from the animal's tissue. The linear range was 0.3-50 ng/g (SC was 0.5-50 ng/g).The precisions (RSD%) were obtained in the range of 2-12% at 2 ng g-1 and 5-15% at 40 ng g-1. The LODs ranged between 2.9-11.7 pg g-1. The LOQs ranged between 9.6-39.1 pg g-1.The proposed method was also successfully applied to the analysis of trace nitrofuran metabolites in animal's tissue.
其他識別: U0005-1007200911053600
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