食品科学 ›› 2005, Vol. 26 ›› Issue (10): 160-165.

• 分析检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定家禽组织中硝基呋喃类抗生素代谢物残留的研究

 庞国芳, 张进杰, 曹彦忠, 范春林, 李学民, 郭彤彤, 曹亚萍, 刘永明   

  1. 秦皇岛出入境检验检疫局
  • 出版日期:2005-10-15 发布日期:2011-09-25

Determination of the Metabolites of Nitrofuran Antibiotics in Poultry Tissues by Liquid Chromatography-Tandem Mass Spectrometry

 PANG  Guo-Fang, ZHANG  Jin-Jie, CAO  Yan-Zhong, FAN  Chun-Lin, LI  Xue-Min, GUO  Tong-Tong, CAO  Ya-Ping, LIU  Yong-Ming   

  1. Qinhuangdao Entry-Exit Inspection and Quarantine Bureau
  • Online:2005-10-15 Published:2011-09-25

摘要: 本文建立了用高效液相色谱-串联质谱(LC-MS-MS)测定禽肉组织中3-氨基-2-唑烷基酮(AOZ)、5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)、氨基脲(SEM)和1-氨基-2-内酰脲(AHD)4种硝基呋喃类抗生素代谢物的方法。0.2mol/L盐酸水解禽肉组织中与蛋白结合的硝基呋喃代谢物,用2-硝基苯甲醛(2-NBA)37℃衍生16h。上清液调pH=7.4后,用LiChrolutEN固相萃取柱净化,乙酸乙酯洗脱,流动相定容。采用电喷雾电离,正离子扫描,多反应监测(MRM)模式检测,标准曲线用空白禽肉样品添加标准与样品同步操作获得并用其进行外标定量。在添加浓度0.5~10μg/kg范围内,四种代谢物的平均回收率在70.2%~89.1%,检出限AMOZ、AOZ为0.1μg/kg,SEM、AHD为0.2μg/kg。10次测定结果相对标准偏差在5.59%~10.10%之间。

关键词: 高效液相色谱-串联质谱, 硝基呋喃类抗生素, 禽肉组织

Abstract: A method for determination of the four metabolites of nitrofuran antibiotics such as 3-amino-2-oxazolidinone (AOZ), 3-amino-5-morpholinomethyl-2- oxazolidinone (AMOZ), semicarbazide (SEM) and 1-aminohydantoin(AHD) in Poultry Tis- sues by LC-MS-MS was developed. Poultry Tissues samples was hydrolyzed with 0.2M HCl, and derivatized at 37℃ for 16h with 2-nitrobenzaldenhyde. The derivatized solutions were adjusted to pH=7.4, and then were cleaned up with LiChrolut EN cartridge, the target compounds were eluted with ethyl acetate and diluted with mobile phase. MS detection was performed in the positive ion mode using multiple reaction monitoring (MRM). The standard calibration curve for four kinds of metabolites were obtained through the synchronized operation of using blank Poultry Tissues sample fortification standard and Poultry Tissues samples for a quantitative analysis per the external standard. In the range of fortification concentration of 0.5~5μg/kg, the average recoveries for these four kinds of metabolites fell within 70.2%~89.1%. Limit of detection for AOZ and AMOZ was 0.1μg/kg, limit of detection for SEM and AHD 0.2μg/kg. The relative standard deviation (CV) was between 5.59%~10.10% (n=10).

Key words: LC-MS-MS, nitrofuran antibiotics, poultry tissues