摘要
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 an ion-exclusion chromatography with direct conductivity detection for the simultaneous separation and determination of salicylic acid and benzoic acid in medicine.Methods：Chromatographic separation was performed on a Shim-pack SCR-102H column with sulfuric acid as the eluent.The influence of the eluent concentration,the column temperature and flow rate of eluent on the retention times of salicylic acid and benzoic acid was investigated.The best chromatographic conditions were as follows：0.04 mmol·L-1 sulfuric acid as eluent,flow rate 1.2 mL·min-1,and column temperature 40 ℃.Rseults：The linear response range of salicylic acid and benzoic acid were 0.5-100 mg·L-1 （ r=0.9999） and 1-100 mg·L-1 （r=0.9999）,respectively.The detection limits were obtained 0.093 mg·L-1 of salicylic acid and 0.32 mg·L-1 of benzoic acid.The relative standard deviations of the chromatographic peak areas were less than 0.4% （n=7）.The method has been applied to the determination of salicylic acid and benzoic acid in the medicine of Zujunqing tinctura and salicylic acid and benzoic acid terpineol liniment with satisfactory results.The recoveries of spiked components of salicylic acid and benzoic acid were 99.5%-100.3% and 99.3%-100.4%,respectively.Conclusion：The method is simple,accurate,reliable and repeatable.It can be applied to the quality control of medicines.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第8期1454-1458,共5页
Chinese Journal of Pharmaceutical Analysis
基金
哈尔滨师范大学科技发展预言项目(No.08XYG-15)
关键词
离子排斥色谱法
水杨酸
苯甲酸
ion-exclusion chromatography
salicylic acid
benzoic acid
