飼料中林可黴素檢驗方法之研發

Research and development of methodology for determining lincomycin residue in animal feed by GC/MS

張凱鈞(Kai-Chun Chang) ； 陳美雲(Mei-Yun Chen) ； 張玉婷(Yu-Ting Chang) ； 蘇忠楨(Jung-Jeng Su)

《台灣農學會報》 13卷1期 (2012/02) Pp. 61-82

摘要

本實驗為應用氣相層析質譜儀開發飼料中林可黴素殘留檢測方法。飼料經5%甲醇溶液萃取及卡瑞試劑沉澱蛋白質後，以hydrophilic-lipophilic balance（HLB）材質之固相萃取管純化，再以N-methyl-N（trimethylsilyl）trifluoroacetamide（MSTFA）衍生化反應，使用內標準品檢量線定量，所得到之結果在0-0.25μg/mL之範圍時具有R^2=0.995之線性回歸方程式，最低偵測極限值為0.01μg/mL，最低定量極限值為0.05μg/mL，方法確效使用10、5及1μg/g三種添加濃度測試，所得回收率分別為85.41、81.45及84.33%，重複性試驗的變異介於5.77-8.51 %之間，再現性試驗之變異介於4.00-13.60%之間，所開發出的方法可成功的應用於飼料中林可黴素的殘留檢驗。

關鍵字

林可黴素 ； 氣相層析質譜儀 ； 飼料

並列摘要

A gas chromatography mass spectrometry method has been developed for determining lincomycin residue in animal feed. The feed samples were extracted with sequential extraction followed by HLB cartridge purification as well as sequential MSTFA derivation. The internal standard curves were notably linear in the range of 0-0.25μg/mL for quantification with a detection limit of 0.01μg/mL and quantification limit of 0.05μg/mL. The recovery percentages for the feed samples were 85.41, 81.45, and 84.33% by the spike experiments at three different concentrations of lincomycin, 10, 5, and 1μg/mg, respectively. In addition, the corresponding inter-day and intra-day precisions were 5.77-8.51 % and 4.00-13.60 %, respectively. Therefore, the successfully developed analytical method might be applied to analyze lincomycin residue in animal feed.

並列關鍵字

Lincomycin ； Gas chromatography mass spectrometry ； Feed