液质联用分析甲锭前体甲基化产物  

Analysis of Methidium's Precursor Methylates by HPLC-MS

作　　者：符迈进[1] 徐霞[1] 艾秀珍[1] 朱京科[1] 

机构地区：[1]浙江大学材料与化工学院化工系,浙江杭州310027

出　　处：《化学世界》2007年第5期272-274,共3页Chemical World

摘　　要：利用反相高效液相色谱-质谱联用方法分析了甲锭前体甲基化产物。以甲醇∶水=75∶25为流动相,流量为0.15 mL/min,在Hypersil ODS(21×100 mm,3μm),检测波长254 nm的色谱条件下分离甲基化目标产物与杂质。采用质谱对甲基化反应液的主要组分进行鉴定,确定了甲基化的主要产物。通过HPLC检测的方法对反应中反应产物的检测,研究表明在反应温度为160℃,反应时间为4 h,甲锭前体与硫酸二甲酯摩尔比为1∶5的条件下,甲锭前体的收率为96.1%,目标产物的纯度可达到92.3%。The analysis of methidium＇ s precursor methylates was carried out by reversed phase liquid chromatography wilh UV and MS detectops. On a Hypersil ODS column, separation was achieved in a methanol： water = 75 ： 25 solvent system. The seven peaks were separated, and four peaks were identified by electrospray mass spectrometry. By studying the reaction, the optimal reaction conditions are reaction temperature with 160 ℃, reaction time with 4 h and the ratio of methidium＇s precursor and DMS with 1 to 5. Under such conditions, the product with purity of 92.3% could be obtained.

关 键 词：液质联用 甲锭 甲基化反应 

分 类 号：O657.6[理学—分析化学]