对甲苯磺酸中间位、邻位同分异构体在高效液相色谱中的分离探究  

Optimization and Separation of Meta-and Ortho-Isomers of p-Toluenesulfonic Acid by High-Performance Liquid Chromatography

作　　者：陈欧 郑晴晴 刘欢 施宗波 卓润生 CHEN Ou;ZHENG Qingqing;LIU Huan;SHI Zongbo;ZHUO Runsheng(Rezel Catalyst Co.Ltd.,Leshan 614000,Sichuan China)

机构地区：[1]润和催化剂股份有限公司,四川乐山614000

出　　处：《分析测试技术与仪器》2024年第5期321-326,共6页Analysis and Testing Technology and Instruments

摘　　要：探究高效液相色谱技术在对甲苯磺酸同分异构体(间位与邻位)分离与定量中的应用.采用Hypercarb(3μm,100 mm×4.6 mm)色谱柱,通过优化流动相(0.1%高氯酸水溶液/乙腈)、柱温(30℃)及检测波长(210 nm)等色谱条件,确立了最佳分离方案.在梯度洗脱模式下,成功实现了对甲苯磺酸间位、邻位同分异构体的高效分离,分离度均超过1.5.进一步基于外标法构建标准曲线,确认了间甲苯磺酸与邻甲苯磺酸分别在0.056~1.12 mg/mL和0.054~1.09 mg/mL范围内具备良好的线性相关性.此外,通过加标回收试验验证,各异构体的回收率稳定在96%~104%之间,且相对标准偏差(RSD)为0.32%~2.02%,充分证明了在定量分析中的准确性和可靠性.The application of high-performance liquid chromatography(HPLC)in the separation and quantification of isomers(meta-and ortho-)of p-toluenesulfonic acid was explored.The optimum separation condition was achieved on a Hypercarb(3μm,100 mm×4.6 mm)column by optimising the mobile phase(0.1%perchloric acid/acetonitrile),column temperature(30℃)and detection wavelength(210 nm).Under the gradient elution mode,the efficient separation of meta-,and ortho-isomers of p-toluenesulfonic acid were successfully achieved,with the resolution exceeding 1.5.Furthermore,the standard curves were constructed based on external standard method,which confirmed that meta-,and ortho-toluenesulfonic acid had good linear correlations in the concentration ranges of 0.056~1.12 mg/mL and 0.054~1.09 mg/mL,respectively.In addition,through the validation test with spiked recovery,the recoveries of the isomers were in the range of 96%~104%,and the relative standard deviations(RSDs)were 0.32%~2.02%,which fully proved the accuracy and reliability of the method in quantitative analysis.

关 键 词：对甲苯磺酸同分异构体 高效液相色谱 定量分析 

分 类 号：O657.7[理学—分析化学]