摘要
研究用高效液相色谱法测定复方苯甲酸软膏的含量。用甲醇做溶剂,70℃水浴溶解软膏,冰浴析出基质,使基质与水杨酸、苯甲酸分离,采用Zorbax-SB C_(18)柱,0.1Mol/L磷酸氢二钠:甲醇(60:40)作为流动相,流速0.8mL/min。在240nm波长处,用外标法测定含量。苯甲酸、水杨酸浓度分别在0.01～0.2mg/mL范围内线性关系良好,R=0.9996。最低检测限为200ng/mL。日内精密度为0.01%～0.04%,0.019%～0.11%,日间精密度为0.045%～0.74%,0.039%～0.19%。方法回收率苯甲酸为:98.31% (n=4),RSD0.79%。水杨酸为:98.54% (n=4),RSD为1.62%。基质凡士林对苯甲酸、水杨酸的测定无干扰。试验证明本方法操作简便、快速,结果准确,可用于该制剂的含量测定。
OBJECTIVE A HPLC method was studied and developed to deternine the content of benzoic acid and salicylic acid in compound benzoic acid ointment simutaneously.METHEDS Methanol as extract solvent, the ointment was soluted in methanol at 70℃ water bath and the addition of ointment was separated by coolling the solution on ice.The separation was carried out on a ZorbaxSB-C_(18) column(4.6mm×250mm,5μm),0.1mol/L Na_2HPO_4:MEOH(60:40,adjust PH 5.2 by phosphoric acid) was used as a mobile phase,at a flow rate of 0.8ml/min. Detection wavelenth was at 240nm.RESULTS The linear range of calibration curve of benzoic acid and salicylic acid were 0.01～0.2mg/mL(r=0.9996).The limits of detection were 200ng/mL.The within-day RSD were 0.01%～0.04%, 0.019%～0.11%,The between-day RSD were 0.045%～0.74%,0.039%～0.19% respectively.The average recoveris of benzoic acid and salicylic acid were 98.31%,RSD=0.79%(n=4) and 98.54%,RSD=1.62%,(n=4).CONCLUSION The method was simple,rapid and accurate.It can be used for the quality control of the compound benzoic acid oinment.
出处
《现代仪器》
2009年第6期72-73,共2页
Modern Instruments
