食品科学 ›› 2005, Vol. 26 ›› Issue (12): 199-201.

• 分析检测 • 上一篇    下一篇

高效液相色谱与质谱联用法分离与鉴定己烯雌酚合成抗原的研究

 朱东辉, 胥传来   

  1. 南通职业大学,江南大学食品学院
  • 出版日期:2005-12-15 发布日期:2011-10-01

Separation and Identification of Synthetic Antigen of Diethylstilbestrol by Using HPLC-MS

 ZHU  Dong-Hui, XU  Chuan-Lai   

  1. 1.Nantong Vocational College;2.School of Food Science and Technology, Southern Yangtze University
  • Online:2005-12-15 Published:2011-10-01

摘要: 采用LichrospherC-18柱,用甲醇和水为流动相,流速0.3ml/min,甲醇从60%~100%梯度洗脱25min,液质联用,电喷雾(ESI),对己烯雌酚及其衍生物己烯雌酚-单(双)-丁酸乙酯基-醚进行了分离和结构鉴定。以混合酸酐法将DES-MCPE与载体蛋白偶联形成完全抗原,并以紫外扫描分析了完全抗原的偶联比率。结果表明:在极性溶剂中,己烯雌酚和其衍生物存在着顺反异构转化现象,极性有机溶剂的溶剂化作用促使顺反异构体的转化。计算DES-MCPE-BSA偶联比率为10。

关键词: 液质联用, 分离, 己烯雌酚, 完全抗原

Abstract: Using liquid chromatography spectrometry (ESI), phase B (methyl alcohol), phase A (water), 0.3mlmin of flow rate, a linear gradient from 60% to 100% of phase B and eluate for 25 minutes on a Lichrospher C-18 column, diethylstilbestrol andi t’sd erivatesc is (tran)- diethylstilbestrol- mno- ether-butyrate-ethyl( DES-MEBE),d iethylstilbestrol-di-ether-butyrate- ethyl (DES-DEBE) were separated and identified. The conjugates of DES-MCPE with proteins as complete antigens were prepared by the mixed anhydride method and the conjugation rate of them were analyzed by UV scanning. The results demonstrated that the isomerization was present in cis and tans of DES and it’s derivates, which was effected obviously by polar solvents. And through calculation the conjugation rate was 10.

Key words: HPLCMS, separation, diethylstilbestrol, synthetic antigen