论文部分内容阅读
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 thiosemicarbazone product were analyzed and identified. A high performance liquid chromatography (HPLC) separation method of thiosemicarbazone and impurities was established. The impurities were prepared. The main impurities were found to be dithiourea and methylthiotetrazole by organic-inorganic-organic-matter (MASS) analysis. The results were further confirmed by infrared spectroscopy and nuclear magnetic resonance spectroscopy. High-performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-MS) was used to determine the peak positions of the two impurities. It was deduced that methylthiotetrazole was converted from bisthiourea during the preparation to give amino sulfur The only impurity in the urea product is the conclusion of dithiourea, avoiding the appearance of “false positives”. The reaction mechanism of bisthiourea to methylthiotetrazole under ammonia was discussed.