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目的:建立同时分离测定药品中水杨酸和苯甲酸的离子排斥色谱-直接电导检测法。方法:以Shim-pack SCR-102H色谱柱为分离柱,H2SO4为流动相,考察了流动相浓度、色谱柱温度、流速对分离和测定水杨酸和苯甲酸的影响,确立最佳色谱条件为0.04mmol·L-1H2SO4做淋洗液,流速1.2mL.min-1,色谱柱温40℃。结果:水杨酸和苯甲酸工作曲线的线性范围分别为0.5～100mg·L-1(r=0.9999)和1～100mg·L-1(r=0.9999);水杨酸的检出限为0.093mg·L-1,苯甲酸的检出限为0.32mg·L-1;相对标准偏差均在0.4%以下(n=7)。将方法应用于足君清酊剂和水杨酸苯甲酸松油搽剂2种药品的分析,获得满意结果,水杨酸和苯甲酸的加样回收率分别为99.5%～100.3%和99.3%～100.4%。结论:本方法简便,结果准确、可靠,重复性好,适用于上述2种药品的质量控制分析。
Objective: To establish a simultaneous separation and determination of salicylic acid and benzoic acid drugs by ion exclusion chromatography - direct conductivity detection method. Methods: Shim-pack SCR-102H column and H2SO4 were used as mobile phases. The effects of mobile phase concentration, column temperature and flow rate on the separation and determination of salicylic acid and benzoic acid were investigated. The optimum chromatographic conditions were 0.04mmol · L-1H2SO4 eluent, flow rate 1.2mL.min-1, the column temperature 40 ℃. Results: The linear range of salicylic acid and benzoic acid working curves was 0.5-100 mg · L -1 (r = 0.9999) and 1-100 mg · L -1 (r = 0.9999) respectively. The detection limit of salicylic acid was 0.093 mg · L-1, and the detection limit of benzoic acid was 0.32 mg · L-1. The relative standard deviations were all below 0.4% (n = 7). The method was applied to the analysis of two kinds of drugs of Zujunqing tincture and benzoic acid pine oil liniment and the satisfactory results were obtained. The recovery rates of salicylic acid and benzoic acid were 99.5% ~ 100.3% and 99.3% ~ 100.4%. Conclusion: The method is simple, accurate, reliable and reproducible. It is suitable for the quality control analysis of the above two drugs.