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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。
The synthesis of 1,4-butanedisulfonic acid disodium salt was studied. In the synthesis of disodium salt of 1,4-butane disulfonate, the best reaction time is about 3 h due to the addition of surfactant EDTA in the reaction system. Compared with 36 h in literature [1] The reaction time is greatly shortened, and the average conversion rate of the reaction is 99.39%. A quantitative method for the determination of 1,4-butanedisulfonic acid by high performance capillary electrophoresis (HPCE) was established. The analytical conditions were as follows: the uncoated capillary column was 50 μm × 81 cm (AGILENT), the buffer solution was 20 mmol borax solution (pH = 9.24), the detection wavelength was 191.2 nm, the voltage was injected and the injection voltage was 30 kV. 5 s. The standard curve, precision, accuracy and reproducibility were studied. The linear correlation coefficient of this method was 0.999, the intra-day coefficient of variation was 0.8%, the intra-day coefficient of variation was 0.5% and the recovery rate was 96.5%. HPCE method has the advantages of high accuracy, good reproducibility, high sensitivity and rapid determination, which is very suitable for the determination of 1,4-butane disulfonate disodium salt content.