HPLC法测定硫糖铝凝胶中3种防腐剂的含量

目的建立测定硫糖铝凝胶中苯甲酸钠、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯3种防腐剂含量的HPLC法。方法采用HPLC法,以C18硅烷键和硅胶为固定相;甲醇-10mL·L-1醋酸溶液(60∶40)为流动相;检测波长为254nm;柱温箱温度为35℃;流速为1.0mL·min-1。结果苯甲酸钠、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯的质量浓度分别在20~200,20~200和2~20μg·mL-1范围内呈良好的线性关系;相关系数分别为0.995 3,0.999 1和0.999 1。3组分在3个不同质量浓度水平的回收率分别为:苯甲酸钠98.7%,100.6%和100.4%;对羟基苯甲酸甲酯97.8%,108.0%和104.8%;对羟基苯甲酸丙酯98.3%,100.5%和100.4%(n=9)。苯甲酸钠、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯的峰面积的RSD值分别为0.05%,0.05%和0.04%(n=6)。结论该方法操作简便、快捷,能够准确检测硫糖铝凝胶中3种防腐剂的含量。

Determination of the content of 3 preservatives in Sucralfate Gels by HPLC

Objective To establish a determination method for 3 preservatives, sodium benzoate,sodium methyl p-hydroxy benzoate,and sodium propyl p-hydroxy benzoate in Sucralfate Gels.Methods HPLC was adopted with C18 bonded silica gels as stationary phase,methanol-10 mL?L-1 acetic acid (60∶40) as mobile phase,254 nm wavelength detecting,along with 35 ℃ column temperature and 1.0 mL?min-1 flow rate.Results This method had good linear correlation when concentrations were within 20-200 μg?mL-1 of sodium benzoate and methyl 4-hydroxybenzoate,as well as within 2-20 μg?mL-1 of propyl 4-hydroxybenzoate.The regression coefficients were 0.995 3,0.999 1 and 0.999 1, respectively.The recoveries of three components at different concentrations were 98.7%,100.6% and 100.4% of sodium benzoate,97.8%,108.0% and 104.8% of methyl 4-hydroxybenzoate,and 98.3%,100.5% and 100.4% of propyl 4-hydroxybenzoate (n=9).Their corresponding precisions RSD were 0.05%,0.05% and 0.04%(n=6).Conclusion This method can be easily manipulated to obtain reliable data of 3 preservatives in Sucralfate Gels.