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目的:建立一种反相离子对高效液相色谱法测定2,5-二羟基苯磺酸盐(包括钙盐、铵盐)的含量及其有关物质。方法:选用Kromasil 100-5C18柱(250 mm×4.6 mm,5μm),以乙腈-甲醇-0.2%磷酸二氢钾溶液(含0.2%四丁基溴化铵,用磷酸调pH为3.10±0.05)(10∶25∶65)为流动相,流速1.0 mL.min-1,检测波长260 nm,柱温30℃。结果:IP-HPLC测定2,5-二羟基苯磺酸钙、2,5-二羟基苯磺酸铵的线性范围均为20.0～500μg.mL-1,相关系数分别为0.9999和0.9998;最低检测限(S/N≥3)分别为1.44和1.64 ng;精密度RSD(n=6)分别为0.21%和0.23%。结论:本法准确、可靠,应用范围广泛。
Objective: To establish a reversed-phase ion pair high performance liquid chromatographic method for the determination of 2,5-dihydroxybenzenesulfonate (including calcium and ammonium salts) and its related substances. METHODS: Kromasil 100-5C18 column (250 mm × 4.6 mm, 5 μm) was used in this study. The samples were eluted with acetonitrile-methanol-0.2% potassium dihydrogen phosphate solution containing 0.2% tetrabutylammonium bromide and adjusted to pH 3.10 ± 0.05 with phosphoric acid (10:25:65) as the mobile phase at a flow rate of 1.0 mL · min-1. The detection wavelength was 260 nm and the column temperature was 30 ℃. Results: The linear ranges of calcium 2,5-dihydroxybenzenesulfonate and 2,5-dihydroxybenzenesulfonate were 20.0-500μg.mL-1 by IP-HPLC with correlation coefficients of 0.9999 and 0.9998 respectively. The lowest detection limit The limits (S / N≥3) were 1.44 and 1.64 ng, respectively; the precision RSD (n = 6) were 0.21% and 0.23% respectively. Conclusion: This law is accurate, reliable and has a wide range of applications.