HPLC法测定硫糖铝凝胶中3种防腐剂的含量

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

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。

To establish a determination method for 3 preservatives, sodium benzoate,sodium methyl p-hydroxy benzoate,and sodium propyl p-hydroxy benzoate in Sucralfate Gels. HPLC was adopted with C18 bonded silica gels as stationaryphase,methanol-10 mL＊L 1 acetic acid （60：40） as mobile phase,254 nm wavelength detecting,along with 35 °C column tempera-ture and 1. 0 mL · min 1 flow rate. This method had good linear correlation when concentrations were within 20-200jug · mL 1 of sodium benzoate and methyl 4-hydroxybenzoate,as well as within 2-20 jug · mL 1 of propyl 4-hydroxybenzoate. The regres-sion coefficients were 0. 995 3,0. 999 1 and 0. 999 1,respectively. T h e 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. 0 5 % and 0. 0 4 % （ n = 6）.This method can be easily manipulated to obtain reliable data of 3 preservatives in Sucralfate Gels.