禽肉和蛋中殺蟲劑賽滅淨和其衍生物蜜胺之高效能液態層析測定   全文下載

High Performance Liquid Chromatographic Determination of Cyromazine and Its Derivative Melamine in Poultry Meats and Eggs

本研究為利用高效能液相層析儀（HPLC）偵測殺蟲劑賽滅淨（cyromazine）及其代謝物蜜胺（melamine）在禽畜產品之殘留量，肉品經鹼處理後，以含20%濃氫氣化銨之乙?萃取，在經Sep-Pak C18固相萃取匣過濾精製得分析樣品，以NH2層析管柱配合移動相為乙?去離子水混合液之梯度溶液比例程式進行分析，顯示兩種成分可在12 min內清晰分離。本方法經多重添加回收試驗結果顯示添加賽滅淨。2~0.7 ppm 檢體濃度，於雞肉、雞蛋、豬肉、牛肉及羊肉中之平均回收率為92.8~97.3%，變異係數為2.2~5.6%。添加蜜胺0.2~0.7 ppm檢體濃度，於雞肉、雞蛋、豬肉、牛肉及羊肉中之平均回收率為91.0~96.1%，變異係數為3.1~7.4%。兩者之標準曲線線性關係良好，線性回歸係數均為 r = 0.999 以訊號／雜訊比 （S／N ratio） 大於3作為判定基準，估算本方法最低檢出限量0.02 ppm。另外依此檢驗方法進行市售禽畜樣品共計46件之調查，結果發現僅1件台灣產牛肉含有0.04 ppm賽滅淨，低於我國殘留限量標準0.2 ppm。此檢體進一步經氣相層析質譜儀確認係為賽滅淨。其他45件檢體均未含有賽滅淨及蜜胺殘留量之檢出，顯示市售禽畜肉產品並沒有賽滅淨殘留之嚴重顧慮。

A high performance liquid chromatography (HPLC) with NH2 column and 75% acetonitrile eluate to determine the insecticide cyromazine residues in poultry meats and eggs was developed. Samples were treated with NaOH, extracted with acetonitrile containing 20% concentrated NH4OH, and cleaned up through C18 Sep-Pak cartridge. The peaks of cyromazine and its metabolite melamine were successfully separated within 12 min and cleanly differentiated from interfering peaks of the samples. The detection limit of both compounds was 0.02 ppm. Recoveries of cyromazine and melamine ranged from 92.8-97.3% and 91.0-96.1% at fortified levels of 0.2- 0.7 ppm, respectively. Each reaction coefficient of linear standard curve of cyromazine and melamine was better than 0.999. Using this HPLC determination, only one beef sample from 46 tested samples was detected to contain 0.04 ppm cyromazine. This was further confirmed by gas chromatography-mass spectroscopy. 本研究為利用高效能液相層析儀（HPLC）偵測殺蟲劑賽滅淨（cyromazine）及其代謝物蜜胺（melamine）在禽畜產品之殘留量，肉品經鹼處理後，以含20%濃氫氣化銨之乙腈萃取，在經Sep-Pak C18固相萃取匣過濾精製得分析樣品，以NH2層析管柱配合移動相為乙腈去離子水混合液之梯度溶液比例程式進行分析，顯示兩種成分可在12 min內清晰分離。本方法經多重添加回收試驗結果顯示添加賽滅淨。2～0.7 ppm 檢體濃度，於雞肉、雞蛋、豬肉、牛肉及羊肉中之平均回收率為92.8～97.3%，變異係數為2.2～5.6%。添加蜜胺0.2～0.7 ppm檢體濃度，於雞肉、雞蛋、豬肉、牛肉及羊肉中之平均回收率為91.0～96.1%，變異係數為3.1～7.4%。兩者之標準曲線線性關係良好，線性回歸係數均為 r = 0.999 以訊號／雜訊比 （S／N ratio） 大於3作為判定基準，估算本方法最低檢出限量0.02 ppm。另外依此檢驗方法進行市售禽畜樣品共計46件之調查，結果發現僅1件台灣產牛肉含有0.04 ppm賽滅淨，低於我國殘留限量標準0.2 ppm。此檢體進一步經氣相層析質譜儀確認係為賽滅淨。其他45件檢體均未含有賽滅淨及蜜胺殘留量之檢出，顯示市售禽畜肉產品並沒有賽滅淨殘留之嚴重顧慮。