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高效液相色谱法同时测定对羟基苯甲酸酯类及对羟基苯甲酸

闫妍,刘永明,朱晓琼   

  1. 东北制药集团股份有限公司,东北制药集团股份有限公司,东北制药集团股份有限公司
  • 收稿日期:2014-01-23 修回日期:2014-04-02 出版日期:2014-04-25 发布日期:2014-04-25

HPLC Method for simultaneous Determination of P-Hydroxybenzoic acid esters and P-Hydroxybenzoic acidYAN yan*, LIU yong-ming. Zhu xiaoqiong (Northeast Pharmaceutical(Shenyang) Science Technology Development Co.Ltd.,Shenyang,Liaoning ,110027,China)

  1. Northeast Pharmaceutical(Shenyang) Science,,
  • Received:2014-01-23 Revised:2014-04-02 Online:2014-04-25 Published:2014-04-25

摘要: 目的 建立同时测定口服液体制剂中羟苯甲酯、羟苯丙酯及其降解产物对羟基苯甲酸的反相高效液相色谱系统,为口服制剂中防腐剂含量控制提供依据。方法 采用反相高效液相色谱法,色谱柱为Luna C18柱(250mm?4.6mm,5μm);以0.1%磷酸溶液为流动相A,以乙腈为流动相B,梯度洗脱;检测波长为254nm;流速为1.0ml/min。结果 羟苯甲酯在24.02~72.02μg/mL范围内,羟苯丙酯在3.04~9.04μg/mL范围内,对羟基苯甲酸在0.28~0.84μg/mL范围内浓度均与峰面积呈良好线性关系,线性方程分别为A=90569C 122945(r=0.9999)、A=86802C 15680(r=0.9999)和A=532.5C-498.6(r=0.9999);平均回收率分别为99.7%、99.8%和98.9%;对羟基苯甲酸检出限为0.10ng结论 该方法简便、准确,可用于口服液体制剂中防腐剂羟苯甲酯、羟苯丙酯及其降解产物对羟基苯甲酸含量测定。

Abstract: objective To establish a HPLC method of simultaneous determination of methyl hydroxybenzoate ,propyl hydroxybenzoate and degradation product P-Hydroxybenzoic acid in oral liquid prepatations .method The Luna C18 was adopted to determinate assay with gradient elution, 0.1% phosphonic acid as the mobile phase A and acetonitrile as the mobile phase B. The detection wavelength was 254nm. Results methyl hydroxybenzoate,propyl hydroxybenzoate and P-Hydroxybenzoic acid were good linear in the range of24.02~72.02μg/mL,3.04~9.04μg/mL and 0.28~0.84μg/mL.The linear equation was A=90569C 122945(r=0.9999),A=86802C 15680(r=0.9999) and A=532.5C-498.6(r=0.9999) respectively. The average recoveries of methyl hydroxybenzoate propyl hydroxybenzoate, P-Hydroxybenzoic acid were 98.1% ,98.5% and 98.8% respectively. The detection limit of P-Hydroxybenzoic acid was 0.10 ng. Conclusion The method is simple and accurate. It can be used to detect methyl hydroxybenzoate ,propyl hydroxybenzoate and degradation product P-Hydroxybenzoic acid in oral liquid prepatations .