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臺灣農業化學與食品科學 Scopus

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篇名 超高液相層析串聯質譜法檢測豬組織中的16種乙型受體素
卷期 52:1
並列篇名 Determination of 16 β-agonists in Pork Tissue by Ultra High Liquid Chromatography/Tandem Mass Spectrometry
作者 黃志能趙偉博於柏伸曾素香高雅敏闕麗卿施養志
頁次 031-047
關鍵字 畜禽產品超高效液相層析串聯質譜儀多重殘留分析乙型受體素Animal productsUltra high liquid chromatography/tandem mass spectrometerMultiresidues analysisβ-agonistsScopusTSCI
出刊日期 201402

中文摘要

本研究建立以超高效液相層析串聯質譜法(ultra high liquid chromatography/tandem mass spectrometer, LC/MS/ MS)利用正離子電灑法以多重反應偵測(multiple reaction monitoring, MRM)模式同時分析豬肉、豬肝及豬腎中16項乙型受體素之檢驗方法。檢體經由0.2 M醋酸鈉緩衝液萃取後,配合酵素水解、酸沈澱蛋白質及陽離子固相萃取匣的淨化處理,其檢液以氮氣吹乾,以5 mM醋酸銨:甲醇(9 : 1, v/v)溶液回溶並經由高速離心後,取上清液,使用ZORBOX RRHD Eclipse Plus C18 Column, 1.8 μm, 3.0 × 100 mm層析管柱,以0.1%甲酸溶液與含0.1%甲酸之乙腈溶液為移動相進行梯度流洗,再以串聯質譜儀分析。並運用內標校正後之基質匹配檢量線(matrix-matched calibration curve)進行定量。結果顯示,豬肉方面,在添加2、5、10 ng/g濃度下,16項藥物之平均回收率為73.9-130.7%,變異係數為4.3-27.2%;內臟方面,在添加10、20、40 ng/g濃度下,16項藥物之平均回收率77.8-135.1%,變異係數為2.7-23.4%。本方法之定量極限為2-10 ng/g。

英文摘要

A method for the analysis of 16 p-agonists in pork, swine liver and swine kidney by ultra high liquid chromatography/tandem mass spectrometer (LC/MS/MS) with electrospray ionization was developed. Data acquisition under MS/MS for each p-agonists was achieved by applying multiple reaction monitoring (MRM). The sample was extracted with 0.2 M sodium acetate buffer, followed by hydrolyzsis with enzymes and protein precipitation with acid. After clarified through cation exchange solid-phase extratction, the analyte was dried with nitrogen gas. After resuspensing in 5 mM ammonium acetate:methanol (9 : 1, v/v), the samples were centrifugated with high speed to obtain supernant. The LC separation was conducted on an ZORBOX RRHD Eclipse Plus C18 Column (1.8 μm, 3.0 × 100 mm) with gradient elution of 0.1% formic acid in water and acetonitrile. The recoveries of 16 p-agonists (2, 5 and 10 ng/g) spiked in pork ranged from 73.9 to 130.7% and the coefficients of variation of all p-agonists were between 4.3 to 27.2%. In swine liver and swine kidney, the recoveries of 16 p-agonists (10, 20 and 40 ng/g) ranged from 77.8 to 135.1% and the coefficients of variation of all p-agonists were between 2.7 to 23.4%. The quantitation limit of the above method is 2 to 10 ng/g.

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