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高效液相色谱与质谱联用法分离鉴定己烯雌酚合成抗原
引用本文:胥传来,彭池方,郝凯,金征宇,王武康. 高效液相色谱与质谱联用法分离鉴定己烯雌酚合成抗原[J]. 精细化工, 2005, 22(10): 781-783
作者姓名:胥传来  彭池方  郝凯  金征宇  王武康
作者单位:江南大学,食品学院,江苏,无锡,214036
基金项目:江苏省自然科学基金(No.CK2004023)
摘    要:采用L ichrospher C-18柱,甲醇和水为流动相,流速0.3 mL/m in,甲醇从60%~100%(体积分数)梯度洗脱25 m in,液质联用,电喷雾(ESI),对己烯雌酚(DES)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。以混合酸酐法将己烯雌酚-单-羧丙基-醚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。计算了DES-MCPE-BSA的偶联比率为10。

关 键 词:液质联用  分离  己烯雌酚  完全抗原
文章编号:1003-5214(2005)10-0781-03
收稿时间:2005-02-02
修稿时间:2005-02-022005-05-31

Separation and Identification of Synthetic Antigen of Diethylstilbestrol by HPLC-MS
XU Chuan-lai,PENG Chi-fang,HAO Kai,JIN Zheng-yu,WANG Wu-kang. Separation and Identification of Synthetic Antigen of Diethylstilbestrol by HPLC-MS[J]. Fine Chemicals, 2005, 22(10): 781-783
Authors:XU Chuan-lai  PENG Chi-fang  HAO Kai  JIN Zheng-yu  WANG Wu-kang
Affiliation:School of Food Science and Technology, Southern Yangtze University, Wuxi 214036, Jiangsu, China
Abstract:Diethylstilbestrol(DES) and its derivatives cis(trans)-diethylstilbestrol-mono(ethyl butyrate)ether(DES-MEBE),diethylstilbestrol-di(ethyl butyrate)ether(DES-DEBE) were separated and identified using liquid chromatography/spectrometry(ESI),phase B(methyl alcohol),phase A(water),flow rate of 0.3 mL/min,a linear gradient from 60% to 100% of phase B and eluating for 25 min on a Lichrospher C-18 column.The conjugates of diethylstilbestrolmonocarboxylpropyl ether(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 result demonstrats that isomerization occur in cis and trans of DES and its derivatives,which is effected obviously by polar solvents.By calculation,the conjugation rate is 10.
Keywords:HPLC/MS    separation    diethylstilbestrol    synthetic antigen
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