【摘要】 研究了合成1,4-丁二磺酸二钠盐的工艺。在1,4-丁二磺酸二钠盐的合成过程中,由于在反应体系中加入表面活性剂EDTA,最佳反应时间只要约3 h,与文献[1]中长达36 h相比,大大缩短了反应时间,反应平均转化率为99.39%。建立了用高效毛细管电泳(HPCE)测定1,4-丁二磺酸的定量分析方法。分析条件为:非涂层毛细管柱为50μm×81 cm(AGILENT),缓冲液:20 mmol硼砂溶液(pH=9.24),检测波长:191.2 nm,电压进样,进样电压30 kV,进样时间5 s。对标准曲线、精密度、准确度及重现性进行了研究。该方法的线性相关系数0.999,日内变异系数0.8%,日间变异系数0.5%,回收率96.5%。HPCE法具有准确性高、重现性好、灵敏度高及快速测定的优点,非常适合于1,4-丁二磺酸二钠盐含量的测定。更多还原

【Abstract】 In this paper,the synthesis process of 1,4-butanedisulphonate disodium salt was studied.The reaction time was shortened from 36 hours in the literature[1] to about only 3 hours in the addition of surfactant EDTA of the reaction system.The product yield is 99.39%.In order to analyze the concentration of 1,4-butanedisulphonate in the reaction system,an analytic method based on the high performance capillaries electrophoresis(HPCE) was established.The analytic conditions were as followings,column: uncoated CE capillaries with 50 μm×81 cm(AGILENT);Buffer: 20 mmol borate with pH=9.24;injecting voltage: 30 kV;injecting time: 5 s;and the wavelength of UV detector: 191.2 nm.Under above conditions,a linear relationship was observed between the concentration of 1,4-butanedisulphonate and absorbance.The precision,recovery and repeatability of the methods were evaluated.The results showed that the linear correlation coefficient for the method was 0.999,and recovery ratio was 96.5%.Coefficients of variation within and between days were 0.8% and 0.5%,respectively.The established analytic method is fast,accurate and repeatable,which has been successfully applied in the synthesis process of 1,4-butanedisulphonate disodium salt.更多还原