液相色谱-质谱对预混饲料水解液中一碘酪氨酸与二碘酪氨酸的检测  

Determination of Monoiodotyrosine and Diiodotyrosine in the Hydrolysate of Premix Feeds with Liquid Chromatography-Mass Spectrometry

作　　者：王宗义[1] 杨文军[1] 张丽英[1] 贺平丽[1] 

机构地区：[1]中国农业大学农业部饲料效价与安全监督检验测试中心,北京100193

出　　处：《分析测试学报》2008年第S1期227-230,共4页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(30771577)

摘　　要：A new LC-MS method has been established for determination of momoiodotyrosine(MIT) and diiodotyrosine(DIT) in the hydrolysate of premix feeds.Samples was hydrolyzed with 4.0 mol·L-1 NaOH for 16 h at 110 ℃,then the hydrolysate was cleaned up with a SPE cartridge and injected directly for LC-MS analysis.Chromatographic separation was performed on a 2.1 mm×150 mm,5 μm particle,C18 column with a mixture of acetonitrile and 0.1%(by volume) acetic acid as mobile phase at a flow rate of 0.2 mL· min-1.ESI+ mass spectrometry detection was run on SIR mode with m/z 308,262 for MIT,and m/z 434,388 for DIT.Quantification was carried out with external standard method.Validation data indicated the method was linear in the concentration ranges investigated with regression coefficients(R2) of more than 0.99.The limits of detection(LOD) were 8 μg·L-1 and limits of quantification(LOQ) were 30 μg·L-1.The recoveries were range of 93%-110% with relative standard deviations of 6.5%-13.2%.The method was sensitive,accurate,and was applied in the determination of MIT and DIT in real sample with satisfactory results.A new LC-MS method has been established for determination of momoiodotyrosine(MIT) and diiodotyrosine(DIT) in the hydrolysate of premix feeds.Samples was hydrolyzed with 4.0 mol·L-1 NaOH for 16 h at 110 ℃,then the hydrolysate was cleaned up with a SPE cartridge and injected directly for LC-MS analysis.Chromatographic separation was performed on a 2.1 mm×150 mm,5 μm particle,C18 column with a mixture of acetonitrile and 0.1%(by volume) acetic acid as mobile phase at a flow rate of 0.2 mL· min-1.ESI+ mass spectrometry detection was run on SIR mode with m/z 308,262 for MIT,and m/z 434,388 for DIT.Quantification was carried out with external standard method.Validation data indicated the method was linear in the concentration ranges investigated with regression coefficients(R2) of more than 0.99.The limits of detection(LOD) were 8 μg·L-1 and limits of quantification(LOQ) were 30 μg·L-1.The recoveries were range of 93%-110% with relative standard deviations of 6.5%-13.2%.The method was sensitive,accurate,and was applied in the determination of MIT and DIT in real sample with satisfactory results.

关 键 词：monoiodotyrosine diiodotyrosine PREMIX feed liquid chromatography-mass SPECTROMETRY 

分 类 号：S816[农业科学—饲料科学]