液相色谱/串联质谱线性组合法测定动物组织中硝基呋喃代谢产物  

Determination of Nitrofuran Metabolites in Animal Tissues by Isotop Dilution Linear Combination High Performance Liquid Chromatography-Mass Sepctrometry/Mass Spectrometry

作　　者：林黎明 林回春 高彦惠[3] 刘心同 田进国[3] 张鸿伟 

机构地区：[1]青岛出入境检验检疫局,青岛266002 [2]胶州市人民医院,胶州266300 [3]山东大学药学院,济南250012

出　　处：《分析化学》2005年第8期1081-1086,共6页Chinese Journal of Analytical Chemistry

基　　金：科技部食品安全重大专项基金资助

摘　　要：研究了对动物组织中4种硝基呋喃类代谢产物AMOZ、AHD、SEM、AOZ的同位素稀释HPLC-MS/MS线性组合分析方法,以2-基苯甲醛作为衍生化试剂,AMOZ-d5、AOZ- 4作内标,用乙酸乙脂提取,用自制的净化试剂净化,以乙腈- 0.1%甲酸为流动相,采用梯度洗脱,可适应不同种类的动物组织样品前处理,15 min可将4种代谢产物完全分离并测定.提出了HPLC-MS/MS多重反应监测线性组合法的原理并进行了验证,回收率为 85%～118%;定量限(LOQ)为0.1 μg/kg;检出限(LOD)为0.03 μg/kg.A method for the determination of metabolites of nitrofuran such as 5-morpholino-3-amino-2-oxazolidone （ AMOZ ）, 1-aminohydantoin （ AHD ）, semicarbazide （ SEM ） and 3-amino-2-oxaolidne （ AOZ ） in animal tissues has been established by isotope dilution high performance liquid chromatography-mass sepctrometry/mass spectrometry. Samples are derivatised using 2-nitrobenzaldehyde, and extracted with ethyl acetale, cleaned up with clean reagent of selfmade with AMOZ-d5, AOZ-d4 as internal standards. The analytes are separated and analysed by gradient elution of acetonitrle and 0.1% fomic acid in 15 minutes.This method is applicable to determine different animal tissues. The principle of linear combinat multiple reaction monitoring is tosted. The ues of isotope internal standard in combination with the simplified sample preparation leads to a sensitive and reliable analysis method. Average recovery is 85% -118% ; The limits of detection are 0.03μg/kg; The limits of quantification are 0.1μg/kg.

关 键 词：液相色谱 串联质谱 线性组合 含量测定 动物组织 硝基呋喃代谢产物 兽药残留 

分 类 号：O657.63[理学—分析化学] TS207.7[理学—化学]