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題名 | 以高效能液相層析儀檢測飼料中之乙烯雌酚=Determination of Diethylstilbestrol in Feed by High Performance Liquid Chromatography |
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作者 | 陳素芬; 劉其和; 郭美月; 蘇杰夫; | 書刊名 | 行政院農業委員會家畜衛生試驗所研究報告 |
卷期 | 41 民95.12 |
頁次 | 頁165-173 |
分類號 | 437.111 |
關鍵詞 | 高效能液相層析儀; 乙烯雌酚; 飼料; High performance liquid chromatography; Diethylstilbestrol; Feed; |
語文 | 中文(Chinese) |
中文摘要 | 本實驗係以高效能液相層析儀配合光二極體偵測器(HPLC/PDA)分析飼料中之乙烯雌酚(diethylstilbestrol)含量,又為避免低濃度時造成誤判,以高效能液相層析質譜儀(HPLC/MS)再確認。飼料樣品以甲醇當萃取液,經震盪、離心、濃縮上清液,殘渣以70%甲醇溶解,應用 OasisRHLB 卡匣去除干擾物質,最後用甲醇沖提,沖提液以高效能液相層析儀檢測。結果顯示,飼料添加0.5ppm、1 ppm、3 ppm、5 ppm,所得回收率為80.8% - 107.5%。若僅以光二極體偵側器檢測時,其最低檢測極限為0.03 ppm,以質譜偵測器檢測時,其最低檢測極限可達0.005 ppm。結果顯示,本研究所開發的高效能液相層析儀檢測飼料中乙烯雌酚之方法便捷、經濟而可行,可成為飼料中乙烯雌酚的檢驗方法之ㄧ。 |
英文摘要 | High performance liquid chromatography equipped with photodiode array detector (HPLC/PDA) was used to measure the quantity of diethylstilbestrol in feed. To prevent the false positive reaction caused by low concentration of diethylstilbestrol in feed, high performance liquid chromatography equipped with mass spectrophotometer (HPLC/MS) was further used as a confirmation test. The samples were prepared by stirring with methanol, followed by a centrifugation step and then an evaporation step. The residual is then dissolved with 70% methanol and the aqueous solution is cleaned by the assay of solid-phase extraction (SPE) using Oasis®HLB to remove the matrix interference, and the eluate was obtained and analyzed by HPLC/PDC or HPLC/MS. The result showed that the average recover rates of diethylstilbestrol in the spiked samples were during the range of 80.8 - 107.5%. The Limit of Detection (LOD) of PDA was 0.03 ppm and the LOD was 0.005 ppm when the MS was used. |
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