HPLC法快速检测苦参素注射液中8种抑菌剂及苯甲醛

目的: 建立快速筛查和同时测定苦参素注射剂中8种抑菌剂(苯甲醇、苯酚、苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)及苯甲醇降解产物——苯甲醛含量的高效液相色谱法。 方法: 应用Welch Materials XB-C₁₈色谱柱(4.6 mm×250 mm,5 μm);流动相为乙腈-0.02 mol·L^-1醋酸铵(冰醋酸调pH至5.0)梯度洗脱,流速1.0 mL·min^-1,检测波长为211 nm(苯甲醇、苯酚),225 nm(苯甲酸),248 nm(苯甲醛),256 nm(山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)。 结果: 9种成分的峰面积与浓度的线性关系良好(r>0.9998),加样回收率为95.6%~102.2%。 结论: 本方法灵敏,快捷,准确,重复性好,可用于注射剂中抑菌剂的快速筛查与含量分析。

Objective: To establish an HPLC method for rapid screening and simultaneous determination of eight preservatives(benzyl alcohol,phenol,benzoic acid,sorbic acid,benzoic acid,4-hydroxy-,methyl ester,benzoic acid,4-hydroxy-,ethyl ester,benzoic acid,4-hydroxy-,propyl ester,benzoic acid,4-hydroxy-,butyl ester)and benzaldehyde from degradation product of benzyl alcohol in oxymatrine injection. Methods: The analysis was performed on Welch Materials XB-C₁₈ column(4.6 mm×250 mm,5 μm)with the mobile phase consisting of acetonitrile-0.02 mol·L^-1ammonium acetate(glacial acetic acid adjustable pH 5.0)in gradient mode.The detection wavelength was set at 211 nm for benzyl alcohol and phenol,225 nm for benzoic acid,248 nm for benzaldehyde and 256 nm for sorbic acid,benzoic acid,4-hydroxy-,methyl ester,benzoic acid,4-hydroxy-,ethyl ester,benzoic acid,4-hydroxy-,propyl ester,¹benzoic acid,4-hydroxy-,butyl ester. Result: Nine constituents showed good linearity(r>0.9998)in the range of the test concentration.The average recoveries of the method were between 95.6% and 102.2%. Conclusion: The method is sensitive,rapid and accurate with good repeatability,which can be used for rapid screening and determination of the content of preservatives in injection.

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[7] EP 6.0. 1281
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