HPLC法测定对甲苯磺酸中同分异构体  

Determination of Isomers in P-toluene Sulfonic Acid by HPLC

作　　者：孙鹏 杨仁明 Sun Peng;Yang Renming(Sichuan Aupone GOOD Pharmaceutical Co.,Ltd.,Chengdu,Sichuan 610097,China)

机构地区：[1]四川奥邦古得药业有限公司,四川成都610097

出　　处：《化工与医药工程》2024年第4期36-43,共8页Chemical and Pharmaceutical Engineering

摘　　要：建立了对甲苯磺酸中同分异构体含量检测的高效液相色谱法,采用Phenomenex Kinetex Biphenyl(150 mm×4.6 mm,5μm)为色谱柱(联苯柱);以pH 2.3磷酸盐缓冲液(0.05 mol/L的磷酸二氢钾溶液,用稀磷酸调节pH值至2.3)-甲醇(95:5)为流动相,等度洗脱;柱温为30℃;流速为0.8 mL/min;检测波长设置为210 nm;进样体积为5μL。采用主成分对照品法对两个异构体杂质进行含量计算,主峰与各异构体杂质峰间分离良好;定量限均不超过0.089μg/mL;邻甲苯磺酸0.089~2.543μg/mL范围内呈良好线性关系(r=10000);间甲苯磺酸在0.088~2.516μg/mL范围内呈良好线性关系(r=0.9999);重复性和中间精密度检出异构体含量RSD值均小于5.0%;加标样品平均回收率(n=9)为98.76%和100.4%;微小改变流速和柱温等色谱条件,对检测结果均无影响。实验结果表明该方法专属性强、准确度高、操作简单、重复性和耐用性好,可作为对甲苯磺酸中同分异构体的控制。To establish an HPLC method or the determination of isomers in p-toluenesulfonic acid.The chromatographic column was Phenomenex Kinetex Biphenyl(150 mm×4.6 mm,5μm);pH 2.3 potassium dihydrogen phosphate solution(0.05 mol/L potassium dihydrogen phosphate solution,adjust pH to 2.3 by phosphoric acid)-methanol(95:5)was used as mobile phase,and iso-elution dilute was performed.The column temperature was 30℃.The flow rate was 0.8 mL per minute.The detection wavelength is 210 nm;The injection volume was 5μL.The isomers were calculated by principal component external standard method and the main peaks were well separated from each impurity peaks.The limits of quantitation were no more than 0.089μg/mL.O-toluenesulfonic acid showed a good linear relationship in the range of 0.089-2.543μg/mL(r=1.0000).M-toluenesulfonic acid showed a good linear relationship in the range of 0.088-2.516μg/mL(r=0.9999).The RSD values of the isomers detected by repeatability and intermediate precision were less than 5.0%.The average recoveries(n=9)were 100.2%and 100.4%.The chromatographic conditions minor change had no influence on the detection results,such as flow rate and column temperature.The experimental results show that the method has strong specificity,high accuracy,simple operation,good repeatability and durability,and can be used to control isomers in p-toluene sulfonic acid.

关 键 词：对甲苯磺酸 同分异构体 HPLC 异构体杂质 含量 

分 类 号：R927.1[医药卫生—药学] R917