HPLC法同时测定复方水杨酸溶液中四组分的含量

目的: 建立高效液相色谱法同时测定复方水杨酸溶液中四组分含量的方法。 方法: 采用Phenomenex Luna C₁₈(250 mm×4.6 mm,5 SymbolmA@m)色谱柱;磷酸三乙胺溶液(取三乙胺4 mL,加水至1000 mL,用磷酸调pH 2.5)-甲醇(45∶ 55)为流动相;检测波长为220 nm;流速为1.0 mL·min^-1。 结果: 水杨酸、间苯二酚、苯酚、水杨酸甲酯分别在0.1378~0.6980 mg·mL^-1(r = 1.0000)、0.03414~0.1707 mg·mL^-1(r =1.0000)、0.0346~0.173 mg·mL^-1(r =1.0000)、0.0395~0.1975 mg·mL^-1(r =1.0000)范围内线性关系良好,3个浓度组间水杨酸平均回收率分别为99.62%(RSD=0.91%)、100.27%(RSD=0.53%)、99.00%(RSD=0.09%),间苯二酚平均回收率分别为102.02%(RSD=0.97%)、101.22%(RSD=0.63%)、98.32%(RSD=0.03%),苯酚平均回收率分别为99.27%(RSD=0.84%)、101.67%(RSD=0.46%)、101.79%(RSD=0.15%),水杨酸甲酯的平均回收率分别为99.87%(RSD=0.94%)、102.09%(RSD=0.67%)、102.59%(RSD=0.31%)。 结论: 本方法简便、快速、准确,为复方水杨酸溶液的质量控制提供了可靠方法。

Objective: To establish an HPLC method for the determination of four components in compound salicylic acid solution at the same time. Method: The Phenomenex Luna C₁₈ (250 mm×4.6 mm,5μm) column was used,the mobile phase consisted of triethylamine phosphate (take triethylamine 4 mL,adding water to 1000 mL,adjust pH to 2.5 with phosphoric acid)–methanol = (45∶ 55),the detection wavelength was 220 nm,the flow rate was 1.0 mL·min^-1. Results: The linearity in the range for salicylic acid,resorcinol,phenol and methyl salicylate were respectively 0.1378-0.6980 mg·mL^-1 (r=1.0000),0.03414-0.1707 mg·mL^-1 (r=1.0000),0.0346-0.173 mg·mL^-1 (r=1.0000),0.0395-0.1975 mg·mL^-1 (r=1.0000),and the average recoveries (n=3) were respectively 99.62% (RSD=0.91%),100.27% (RSD=0.53%),99.00% (RSD=0.09%);102.02% (RSD=0.97%),101.22% (RSD=0.63%),98.32% (RSD=0.03%);99.27% (RSD=0.84%),101.67% (RSD=0.46%),101.79% (RSD=0.15%);99.87% (RSD=0.94%),102.09% (RSD=0.67%),102.59% (RSD=0.31%). Conclusions: The method was found to be simple and accurate for simultaneous analysis of the content of 4 components in compound salicylic acid solution,and provided a reliable way for the quality control.