【摘要】 通过液相色谱法、核磁共振法、红外光谱法、质谱法对DCJTB产品进行定性检测,结果表明目标产物是trans-DCJTB,关键杂质是cis-。HPLC条件:色谱柱Synergi 4μHydro-RP 80A(150×4.6 mm),二极管阵列检测器,流动相为体积比较65:35的四氢呋喃(THF)/水溶液。NMR条件:标准脉冲序列检测1H NMR,观测频率500.13MHz,内标为四甲基硅烷(δ0)。IR条件:光谱范围4000～400 cm-1,分辨率4 cm-1。MS条件:离子源温度200℃,扫描质量范围(m/z)20～500,进样杆以40℃/min从50℃升至350℃。用HPLC定量:检测波长360 nm,试样用THF溶解。实验表明,在溶解状态下trans-DCJTB不稳定,光照能加速trans-部分转化为cis-。试样溶液在室内自然光照射下放置50 min后trans-纯度从99.2%变为92.2%,若严格避光则50 min后为99.1%,故整个操作应严格避光并在50 min内完成。更多还原

【Abstract】 Qualitative analysis of DCJTB product by HPLC,NMR,IR and MS was performed.Results showed that the target product was trans-DCJTB and the key impurity was cis-.HPLC conditions were as follows: a Synergi 4μ Hydro-RP 80A column(150 × 4.6 mm),a diode-array detector and the mobile phase of THF/H2O = 65 /35.NMR conditions: standard pulse sequence test 1H NMR,an observation frequency of 500.13MHz,an internal standard of TMS(δ0).IR conditions: a spectral region of 4000 cm-1-400 cm-1,a resolution of 4 cm-1.MS conditions: a IE temperature of 200 ℃,scan mass range(m/z) 20-500,injecting pole heated from 50 ℃ to 350 ℃ with 40℃/min.The quantitative determination was measured by HPLC,the detection wavelength was 360 nm,and the sample was dissolved by THF.The trans-DCJTB could be changed into cis-in a solution,and the light could speed the reaction.The purity of sample solution changed from 99.2% to 92.2% even under the indoor daylight in 50 min,on the contrary,the data only turned to 99.1% if the solution was shaded strictly from the light at the same time.So the whole quantitative test operation had to avoid light and be finished within 50 min.更多还原