液相層析串聯式質譜儀檢測牛乳中抗生素化合物

本研究係以具選擇性及靈敏度之高效率液相層析串聯式質譜儀（LC/MS/MS）搭配固相萃取（SPE）與液－液萃取（LLE）技術，建立牛乳中四環黴素類（TCs含TC、CTC及OTC）、氯黴素類（CAPs含CAP、TAP及FF）及青黴素類（PENs含AMOX、AMPI、PENG、CLOX及OXA）殘留量監測分析方法。使用三段式四極棒質譜儀搭配渦輪噴灑離子源在陽離子模式下偵測TCs及PENs，陰離子模式下偵測CAPs。TCs之方法偵測極限（MDL）為1.33～2.73ng/mL，CAPs之MDL為0.048～0.07ng/mL，PENs之MDL為0.90～1.86ng/mL。於允許最大殘留量濃度下，TCs回收率82.04～87.68%，變異係數（CV）2.15～4.53%；TAP及FF回收率68.66～85.10%，CV8.77～10.58%；PENs回收率59.14～76.51%，CV10.11～11.43%。於0.3ng/mL濃度下，CAP回收率109.9%，CV5.89%。本方法可應用於牛乳中TCs、CAPs及PENs等抗生素殘留量分析。

關鍵字

牛乳；四環黴素；氯黴素；青黴素；高效率液相層析串聯式質譜儀

並列摘要

The purpose of this study was to develop a specific and sensitive high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) method with solid-phase extraction (SPE) and liquid-liquid extraction (LLE) for the determination of tetracyclines (TC, CTC and OTC), chloramphenicols (CAP, TAP and FF) and penicillins (AMOX, AMPI, PEN G, CLOX and OXA) residues in milk. A triple-quadruple mass spectrometry using a TurboIon Spray source operating in the positive ion mode was used to detect TCs and PENs, while the negative ion mode was used to detect CAPs. The method detection limit (MDL) for TCs were 1.33～2.73 ng/mL. MDL for CAPs were 0.048～0.07 ng/mL. MDL for PENs were 0.90～1.86 ng/mL. At maximum residue limit level, recoveries of TCs were between 82.04 and 87.68%, with coefficient of variation (CV) ranging between 2.15 and 4.53%. Recoveries of TAP and FF were between 68.66 and 85.10%, with CV ranging between 8.77 and 10.58%. Recoveries of PENs were between 59.14 and 76.51%, with CV ranging between 10.11 and 11.43%. At the 0.3 ng/mL level, recovery of CAP was 109.9%, with a CV of 5.89%. We concluded that the method could be applied to the analysis of TCs, CAPs and PENs residues in milk.

並列關鍵字

Milk ； Tetracyclines ； Chloramphenicols ； Penicillins ； High performance liquid chromatography tandem mass spectrometry

主題瀏覽