以液相層析串聯質譜儀建立牛、羊組織中動物用藥Closantel殘留之檢驗方法

Method Development of Closantel Residues in Bovine and Ovine Tissues by Liquid Chromatography-Tandem Mass Spectrometry

10.6578/TJACFS.202406_62(2).0001

曾衡宇(Heng-Yu Tseng)；黃志能(Chih-Neng Huang)；彭冠智(Guan-Jhih Peng)；林汝青(Nu-Ching Lin)；高雅敏(Ya-Min Kao)；曾素香(Su-Hsiang Tseng)；王德原(Der-Yuan Wang)

Closantel ； 液相層析串質譜儀 ； 乙飽和正己烷 ； 基質匹配檢量線 ； Closantel ； LC-MS/MS ； n-Hexane saturated with acetonitrile ； Matrix-matched calibration curve

臺灣農業化學與食品科學

62卷2期（2024 / 06 / 01）

55 - 62

繁體中文;英文

本研究以液相層析串聯質譜儀建立牛、羊組織中肌肉、內臟、脂肪中之動物用藥closantel之檢驗方法。檢體均質後採用乙腈：丙酮（60：40, v/v）溶液萃取，並以乙飽和正己烷淨化。分離上採用CORTECS C18管柱配合含0.1%甲酸之甲醇溶液及0.1%甲酸溶液進行梯度沖提。分析上採用內部標準品校正之基質匹配檢量線進行定量。本研究進行三個濃度（0.025、0.25及0.5 ng/g）之添加回收試驗，結果顯示，同日中肌肉類檢體之平均回收率介於82.5～104.6%、內臟類檢體之平均回收率介於77.8～110.4%、脂肪之平均回收率介於92.9～100.6%；上述基質中，同日及異日變異係數均小於15%。方法定量極限為0.025 ng/g。

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to determin closantel in muscles, viscera, and fat in bovine and ovine tissues. The homogenized samples were extracted with acetonitrile:acetone (60 : 40, v/v) solution. The extract were further cleaned by n-hexane saturated with acetonitrile. A CORTECS C18 column was used to separate the analyte. Mobile phase consisted of methanol conatining 0.1% formic acid and 0.1% formic acid. Quantitation was performed by matrix-matched calibration curve normalized by internal standard. Recoveries at 0.025, 0.25 and 0.5 ng/g spiking levels ranged from 82.5 to 104.6% in muscles, from 77.8 to 110.4% in viscera, from 92.9 to 100.6% in fat. The intraday precisions and the interday precisions were below 15%. The quantitation limit of the method is 0.025 ng/g.