气相色谱法同时测定中药糖浆剂中3种防腐剂含量

Simultaneous determination of preservatives content in Chinese herb syrups by gas chromatography

关键词:  色谱法  气相  防腐剂  糖浆剂

Key words:  chromatography  GC  preservatives  syrups

摘要:

[目的] 建立中药糖浆剂中苯甲酸、山梨酸、对羟基苯甲酸乙酯等3种常用防腐剂的同时测定方法。[方法] 样品经甲醇溶解、超声提取、离心,采用大口径非极性毛细管色谱柱DB-1(30 m×0.25 mm×0.25 μm)气相色谱法进行定性和定量分析,并探讨最佳实验条件。[结果] 该方法的线性范围为山梨酸10～100 μg/mL,苯甲酸10～100 μg/mL;对羟基苯甲酸乙酯5～50 μg/mL,其相关系数在0.996 9～0.997 9之间,方法最低检出限分别为1.2、1.8、0.7 μg/mL,样品加样回收率为95.4%～103.7%,相对平均偏差为2.9%～3.7%.并成功应用该方法检测实际样品中的防腐剂。[结论] 该方法简易可行,并能较好地分离上述3种化合物,具有分析时间短、抗干扰性好、定量准确等优点。

Abstract:

[Objective] To establish a method for determination of 3 preservatives, benzoic acid, sorbic acid and ethyl-paraben in Chinese herb syrups simultaneously by gas chromatography. [Methods] The Chinese herb syrups sample was dissolved by methanol, extracted by ultrasonic and separated by packed column of DB-1(30 m×0.25 mm×0.25 μm). [Results] The concentrations of 3 preservatives showed a positive correlation with the peak heights at 10～100 μg/mL for sorbic acid, 10～100 μg/mL for benzoic acid and 5～50 μg/mL for ethyl-paraben. The correlative coefficients were 0.996 9～0.997 9. The detection limits were 1.2, 1.8 and 0.7 μg/mL respectively. The recovery rates were 95.4%～103.7%. RSDs were 2.9%～3.7%. [Conclusion] The present method mentioned above can perfectly separate these three preservatives with some advantages, such as simple, accurate, sensitive and quick.