Ding Tao, Xu Jinzhong, Shen Chongyu, Wu Bin, Chen Huilan, Zhu Chun, Zhao Zengyun, Jiang Yuan, Liu Fei
National Bee-Product Reference Laboratory, Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China.
Se Pu. 2006 Sep;24(5):432-5.
Nitrofurans are a group of widely used veterinary antibiotics that have been banned in many countries. This has generated a great deal of interests and demands for assay of nitrofurans in animal food products. To our knowledge, this is the first time that a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method has been successfully developed for simultaneously analyzing the metabolites of four nitrofuran antibiotics (furazolidone, furaltadone, nitrofurazone and nitrofurantoin) in royal jelly. Trichloroacetic acid solution was used both to precipitate proteins and to provide acidic reaction condition. Four isotope internal standards were utilized to improve the quantitative precision. The limits of detection (LODs) were 0.03 microg/kg for the metabolite of furaltadone and 0.05 microg/kg for the other three metabolites. The limits of quantitation were 0.20 microg/kg for the metabolite of furaltadone and 0.25 microg/kg for the other three metabolites. The linear range was 0.4-20 ng/mL for all the target analytes. The recoveries calibrated by internal standard were in the range of 97.7%-104.8 with the relative standard deviations (RSDs) of 2.7-9.7. It showed that this method could meet the requirements of national monitoring plan in China and the Minimum Required Performance Limits (MRPL) set by the European Union.
硝基呋喃是一类广泛使用的兽用抗生素,已在许多国家被禁用。这引发了人们对动物食品中硝基呋喃检测的极大兴趣和需求。据我们所知,这是首次成功开发出一种高效液相色谱 - 串联质谱(HPLC - MS/MS)方法,用于同时分析蜂王浆中四种硝基呋喃抗生素(呋喃唑酮、呋吗唑酮、呋喃西林和呋喃妥因)的代谢物。三氯乙酸溶液既用于沉淀蛋白质,又用于提供酸性反应条件。使用四种同位素内标来提高定量精度。呋喃他酮代谢物的检测限为0.03微克/千克,其他三种代谢物的检测限为0.05微克/千克。呋喃他酮代谢物的定量限为0.20微克/千克,其他三种代谢物的定量限为0.25微克/千克。所有目标分析物的线性范围为0.4 - 20纳克/毫升。以内标校准的回收率在97.7% - 104.8%范围内,相对标准偏差(RSD)为2.7% - 9.7%。结果表明,该方法能够满足中国国家监测计划以及欧盟设定的最低所需性能限度(MRPL)的要求。