氨基硫脲中杂质的鉴定及其反应机理探讨  

Identification and mechanism investigation of the impurities in thiosemicarbazide

作　　者：马浩[1] 尹雪梅[1] 刘娟[1] 姚宝龙[1] 施超欧[1] 

机构地区：[1]华东理工大学分析测试中心,上海200237

出　　处：《分析试验室》2014年第4期474-478,共5页Chinese Journal of Analysis Laboratory

摘　　要：对氨基硫脲产品中的杂质进行了分析和鉴定。建立了氨基硫脲及杂质的高效液相色谱(HPLC)分离方法。对杂质进行制备,有机质谱分析发现杂质主要为双硫脲和甲硫基四氮唑;采用红外光谱(IR)和核磁共振波谱(NMR)进行进一步确定。应用高效液相色谱电喷雾质谱联用法(HPLC-MS)确定了两种杂质的出峰位置,推断出甲硫基四氮唑是在制备过程中由双硫脲转化而来,得出氨基硫脲产品中的杂质只有双硫脲的结论,避免了"假阳性"的出现。探讨了双硫脲在氨水条件下生成甲硫基四氮唑的反应机理。The impurities in the thiosemicarbazide product were determined and analyzed. Firstly, a method was developed to separate the product and impurities by high performance liquid chromatography （HPLC）, and it was found that the impurities were bisthiourea and methylthio-tetrazole mixture by using organic mass spectrometry, and the result was further confirmed by adopting infrared spectroscopy （IR） and nuclear magnetic resonance （NMR）. Through HPLC-MS, the peak positions of two kinds of impurities were detected, and it was deduced that methyhhio-tetrazole was produced in the process of preparation. The conclusion that bisthiourea was the only impurity in thiosemicarbazide products was drawn and ＂false positive＂ was avoided. The reaction mechanism that the main component of the impurities in the product is bisthiourea was firstly explored. The study provides a guiding role for thiosemicarbazide production process.

关 键 词：氨基硫脲 剖析 双硫脲 甲硫基四氮唑 制备 

分 类 号：O657.63[理学—分析化学]