固相萃取高效液相色谱-质谱法测定动物组织中硝基呋喃代谢产物

Determination of Nitrofuran Metablolites in Animal Tissues by High Performance Liquid Chromatography-Mass Spectrometry and Study of Their Residual Discipline

研究了对动物组织中4种硝基呋喃类代谢产物AOZ、AMOZ、SEM和AHD的自动固相萃取HPLCMS分析方法,分别以2氯苯甲醛和2硝基苯甲醛作为衍生化试剂,分别用AMOZd5、AOZd4作内标,用ENSPE柱进行提取,以乙腈0.1%甲酸为流动相,采用梯度洗脱,可在15min内将4种代谢产物完全分离并进行测定。回收率为85%～90%;检出限可达0.5μg/kg。采用两种衍生化方法可获得较多的定性确证信息。采用本方法研究了硝基呋喃在鸡饲养过程中的残留规律。

A liquid chromatography-mass spectrometris method was developed for the simultameous determination of the metablolites of nitrofuran antibacterial drugs such as 3-amino-2-oxaolidone (AOZ), 5-mopholino-3-amino-2-oxazolidone (AMOZ) semicabazide (SEM) and 1-aminohydantion (AHD) in animal tissues. Samples were derivatised using 2-chlorobenzaldehyde or 2-nitrobenzaldehyde, and using AMOZ-6, AOZ-d4 as internal standards cleaned up with EN SPE columns and determined by high performance liquid chromatography-mass spectrometry. The analytes were separated and analysed by gradient elution of acetonitrle and 0.1 % fomic acid in 15 minutes. The recoveries ranged from 85. 0% to 90. 0% and the detection limit was 0. 5 mu g/kg. More identified information is available by using two different derivative methods. Furthermore, the regulation of nitrofuran residues in chick feeding was studied.