Rodziewicz Lech, Zawadzka Iwona
Pracownia Badań Chemicznych Srodków Spozywczych Zakład Higieny Weterynaryjnej 15-959 Białystok, ul. Zwycigstwa 26a.
Rocz Panstw Zakl Hig. 2007;58(4):625-32.
A LC-MS-MS method is presented to analyze simultaneously the metabolites of four nitrofuran veterinary drugs in animal muscle tissue e.g., furazolidone, furaltadone, nitofurantoina and nitrofurazone. The sample clean up were performed by a liquid-liquid extraction with ethyl acetate, after a hydrolysis and derivatization with 2-nitrobenzaldehyde. Nitrofurane metabolites were determined by LC-ESI-MS/MS in positive mode. The LC was equipped with column Luna C18 Phenomenex. A binary gradient mobile phase was used as methanol solvent B containing 0.5 mM ammonium acetate and methanol (80:20 v/v). The method was validated according to criteria of Decision Commission No 2002/657/EC. Samples were fortified with metabolites of nitrofuran between 0.5-2.0 microg/kg with AOZ-d4, and AMOZ-d5 as internal standard. The mean recoveries from meat spiked at 1.0 microg/kg were 84.5-109.7%. Limit of decision (CCalpha) was between 0.25-0.57 and capability of detection (CCbeta) 0.32-0.77 microg/kg.
本文提出了一种液相色谱-串联质谱法,用于同时分析动物肌肉组织中四种硝基呋喃类兽药(如呋喃唑酮、呋吗唑酮、硝呋妥因和呋喃西林)的代谢物。样品在经过水解并用2-硝基苯甲醛衍生化后,通过乙酸乙酯液-液萃取进行净化处理。硝基呋喃代谢物采用液相色谱-电喷雾串联质谱法在正离子模式下测定。液相色谱配备Phenomenex Luna C18色谱柱。二元梯度流动相采用含有0.5 mM乙酸铵的甲醇作为溶剂B,与甲醇(80:20 v/v)混合。该方法根据欧盟委员会第2002/657/EC号决定的标准进行了验证。样品用AOZ-d4和AMOZ-d5作为内标,添加浓度为0.5 - 2.0 μg/kg的硝基呋喃代谢物。在1.0 μg/kg加标的肉样中,平均回收率为84.5 - 109.7%。决策限(CCα)在0.25 - 0.57之间,检测能力(CCβ)为0.32 - 0.7 μg/kg。 (注:原文中“capability of detection (CCbeta) 0.32 - 0.77 microg/kg”疑有误,根据前文及语境推测应为“0.32 - 0.7 μg/kg”,译文已按此修正)