HPLC法测定对氨基苯磺酸钠中的同分异构体

Determination of isomers in sodium sulfanilate by high performance liquid chromatography

目的 建立测定对氨基苯磺酸钠中邻、间氨基苯磺酸钠的HPLC法。方法 METROSEP A SUPP5色谱柱(150 nm×4.0 nm,5μm,METROHM),流动相为0.006 5 mol·L^(-1)碳酸钠溶液-甲醇(90∶10),有关物质等度洗脱,体积流量为0.6 mL·min^(-1),检测波长为240 nm,柱温为30℃,进样量为5μL。考察所建立方法的系统适用性、专属性、定量限、检测限、精密度(重复性和中间精密度)、线性、准确度、溶液稳定性和耐用性。结果 建立的HPLC法系统适用性、专属性良好;邻、间氨基苯磺酸钠分别在0.005~0.050μg·mL^(-1)具有良好的线性关系;检测限、定量限、精密度、线性、准确度、溶液稳定性和耐用性均符合要求。3批对氨基苯磺酸钠中均未检测出间氨基苯磺酸钠和邻氨基苯磺酸钠。结论 该方法灵敏、简单,且专属性高,为实现邻、间氨基苯磺酸钠的准确定量提供了依据。

Objective To establish a HPLC method for the determination of sodium o-aminobenzene sulfonate and sodium maminobenzene sulfonate in sodium p-aminobenzene sulfonate.Methods An METROSEP A SUPP5 column(150 nm × 4.0 nm,5 μm,METROHM) was used.Mobile phase:0.006 5 mol·L^(-1) sodium carbonate solution:methanol(90:10).Isocratic elution was used for the determination of related substances and the flow rate was 0.6 mL·min^(-1).The detection wavelength was 240 nm and the column temperature was maintained at 30 ℃.The injection volume was 5 μL.Results The established HPLC system had good applicability and specificity.The linear relationship between o-aminobenzene sulfonate and m-aminobenzene sulfonate was 0.005—0.050 μg·mL^(-1),respectively.Detection limit,quantitative limit,precision,linearity,accuracy,solution stability and durability all meet the requirements.M-aminobenzene sulfonate and o-aminobenzene sulfonate were not detected in three batches of sodium paminobenzene sulfonate.Conclusion The method was sensitive,simple and specific,which provides the basis for the accurate quantification of sodium o-aminobenzene sulfonate and sodium m-aminobenzene sulfonate.