Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Kasetsart University, Bangkok 10903, Thailand.
J Agric Food Chem. 2009 Mar 11;57(5):1752-9. doi: 10.1021/jf803423r.
The synthesis of derivatives of metabolites from furazolidone, furaltadone, nitrofurazone, and nitrofurantoin using a new derivatizing reagent, 2-naphthaldehyde (NTA), is described. The reaction product was used in liquid chromatography with diode array detector (LC-DAD) for determination of protein-bound metabolites of nitrofurans in shrimp followed by two steps of liquid-liquid extraction. Derivatives of nitrofuran metabolites are well separated from NTA remaining in the extract upon separation on a ChromSpher 5 Pesticide (250 x 4.6 mm, 5 microm) column at 40 degrees C with acetonitrile/5 mM ammonium acetate adjusted to pH 7.5 gradient as the mobile phase and DAD detection at 308 nm except for naphthyl derivative of 1-aminohydantoin at 310 nm. The high absorptivity of these derivatives makes simultaneous screening of these metabolites in shrimp at 1 microg/kg possible for the first time using LC-DAD. The method was validated using blank shrimp fortified with all four metabolites at 1, 1.5, and 2 microg/kg. Recoveries were >86% with relative standard deviations of <14% for all four metabolites. Comparison between LC-DAD and APCI-MS/MS shows very good agreement for shrimp samples.
描述了使用一种新的衍生化试剂 2-萘醛（NTA）合成呋喃唑酮、呋喃它酮、呋喃妥因和呋喃西林代谢物的衍生物。反应产物用于液相色谱-二极管阵列检测器（LC-DAD）测定虾中硝基呋喃的蛋白结合代谢物，然后进行两步液-液萃取。在 40°C 下，用 ChromSpher 5 农药（250 x 4.6 毫米，5 微米）柱分离，以乙腈/5 mM 乙酸铵调节 pH 值至 7.5 梯度作为流动相，DAD 在 308nm 处检测，除了 1-氨基脲的萘基衍生物在 310nm 处检测，硝基呋喃代谢物的衍生物与提取物中残留的 NTA 很好地分离。这些衍生物的高吸光度使得首次能够使用 LC-DAD 在虾中同时筛选这些代谢物，浓度为 1μg/kg。该方法使用空白虾在 1、1.5 和 2μg/kg 水平上添加所有四种代谢物进行验证。四种代谢物的回收率均>86%，相对标准偏差均<14%。LC-DAD 和 APCI-MS/MS 之间的比较表明虾样品之间非常吻合。
