摘要
目的:建立离子色谱法测定4-氯-3-磺酰胺苯甲酸中残留氯磺酸含量的方法。方法:用高纯水溶解样品作为供试品溶液,使用离子色谱仪测定4-氯-3-磺酰胺苯甲酸溶液中氯磺酸所转化的SO_4^(2-) 离子的含量,再换算成对应的氯磺酸残留量。使用Dionex,ICS-90A阴离子分析柱(250mm×4.0mm,5μm),以475mg·L^(-1)碳酸钠和120mg·L^(-1)碳酸氢钠纯水溶液为流动相,流速1.0m L·min-1,运行20分钟;进样量20μL。结果:试验中,专属性溶液产生的色谱数据,与标准溶液与样供试品溶液的色谱数据相比,硫酸根离子的面积明显增加,且硫酸根的离子峰与其他离子峰可以显著分离出来,硫酸根离子峰与最近的离子峰之间的分辨度可达5.887,通过离子交换色谱方法检测4-氯-3-磺酰胺苯甲酸中氯磺酸转化的硫酸根离子,其专属性得到了证实。6份精密度溶液所测保留时间的RSD不大于2.0%,6份精密度溶液所测面积的RSD不大于10%。氯磺酸LOQ的绝对浓度是4.488×10^(-4)mg/m L,相对浓度为22.4ppm。氯磺酸的LOD的绝对浓度是1.122×10^(-4)mg/m L,相对浓度为5.6ppm(S/N约为10:1)。6份LOD溶液测出的峰面积的RSD不超过10%。结论:本法可精确测定4-氯-3-磺酰胺苯甲酸及相关药物中氯磺酸转化的SO_4^(2-) 离子的含量,并能计算出残留氯磺酸含量,有效控制其质量。
To establish an HPIC method for the detection of residual Chlorosulfuric acid in 4-Chloro-3-sulfamoylbenzoic acid.Methods： The sample is resolved by high purity water to prepare the sample solution. The content of ion SO_4^（2-） due to the change of the Chlorosulfuric acid in 4-Chloro-3-sulfamoylbenzoic acid solution is measured by Dionex, ICS-90 A ion chromatography, then the content of residual Chlorosulfuric acid can be analyzed by the conversion of the relative content of ion SO_4^（2-） . The Dionex, Ion Pac TM, AS22 anion analytical column（250 mm×4.0 mm,5 μm） was used with the water solution of 475 mg·L^（-1） sodium carbonate and 120 mg·L^（-1） sodium bicarbonate as the eluent, the flow rate was 1.0 m L·min-1 with the run time of 20 min,the injection volume was 20 μL. Results： In the chromatogram of specificity solution, compared to that of standard solution and sample solution, the peak area of Sulfate ion（SO_4^（2-） ）is apparently increased, and the peak of Sulfate ion（SO_4^（2-） ） is separated from that of other ion. The resolution between Sulfate ion（SO_4^（2-） ） peak and its nearest peak is 5.887. And the specificity of Sulfate ion（SO_4^（2-） ） in 4-Chloro-3-sulfamoylbenzoic acid for the established HPIC method is acceptable. In respect of the precision, RSD of retention time of 6 replicates of solutions is lessthan2.0%.RSD of peak area of 6 replicates of solutions is less than 10.0%. LOQ absolute concentration of Chlorosulfuric acid is4.488 ×10-4 mg/mL, with relative concentration 22.4 ppm. LOD absolute concentration of Chlorosulfuric acid is 1.122 ×10-4 mg/mL, with relative concentration 5.6 ppm. In respect of LOQ repeatability, RSD of peak area of 6 replicates of LOQ solutions is less than 10.0%. Conclusion： The method can accurately detect Residual Chlorosulfuric acid in4-Chloro-3-sulfamoylbenzoic acid, by the conversion of the measurement of ion SO_4^（2-） due to the change of the Chlorosulfuric acid in 4-Chloro-3-sulfamoylbenzoic acid solution, and can be used as an effective method for the quality control of Residual Chlorosulfuric acid.
出处
《科教文汇》
2017年第36期175-180,共6页
Journal of Science and Education
基金
苏州卫生职业技术学院资助课题:离子色谱法分析药物中的氯磺酸残留(编号:szwzy201403)
