HPLC测定对羟基苯甲酸甲酯钠的含量及有关物质

Determination of Content and Related Substances of Methylparaben Sodium by HPLC

关键词:  对羟基苯甲酸甲酯钠  含量测定  有关物质  高效液相色谱法

Key words:  methylparaben sodium  content determination  related substances  HPLC

摘要:

目的 建立对羟基苯甲酸甲酯钠的含量测定及有关物质检查方法。方法 采用高效液相色谱法，色谱柱为Shim-pack VP-ODS C₁₈柱(250 mm×4.6 mm，5 mm)，以甲醇-1%醋酸溶液(60∶40)为流动相，流速1.0 mL·min^-1，柱温35 ℃，波长254 nm。结果 对羟基苯甲酸甲酯与各主要杂质及强制破坏产生的降解产物的杂质峰均分离良好，对羟基苯甲酸甲酯在21.64~194.8 mg·mL^-1内与峰面积呈良好线性关系，r＝1.000，回收率为99.5%(RSD=0.64%，n=9)，最低检出限为0.214 4 ng；供试品溶液在24 h内稳定。结论 本法专属性强，准确、灵敏，方法可靠，可用于对羟基苯甲酸甲酯钠的含量测定和有关物质检查。

Abstract:

OBJECTIVE To establish a method to determine the content and related substances of methylparaben sodium. METHODS HPLC was adopted on a Shim-pack VP-ODS C₁₈ column (250 mm×4.6 mm, 5 μm) using an isocratic mobile phase consisting of methanol-0.1% acetic acid solution (60∶40) with a flow rate of 1.0 mL·min^-1. The column temperature was kept at 35 ℃ and the detection wavelength was set at 254 nm. RESULTS The separation of methyl parahydroxybenzoate and other impurities was achieved within four times of the major peak retention time. The concentration-response relationship was linear over the range of 21.64-194.8 mg·mL^-1(r=1.000). The average recovery was 99.5%(RSD=0.64%, n=9) and the limit of detection was 0.214 4 ng. The solution was stable for 24 h. CONCLUSION The method is specific, accurate, sensitive and suitable for the determination of content and related substances of methylparaben sodium.