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。
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.
出处
《科技通报》
2006年第6期737-741,共5页
Bulletin of Science and Technology
基金
浙江省科技厅科技基金项目
