胶束电动毛细管电泳法同时测定麻杏止咳糖浆中的6种防腐剂

Simultaneous Determination of Six Preservatives in Maxing Zhike Syrup by MEKC-DAD

关键词:  胶束电动毛细管电泳  麻杏止咳糖浆  苯甲酸  山梨酸  苯甲酸甲酯类

Key words:  MEKC-DAD  maxing zhike syrup  benzoic acid  sorbic acid  parabens

摘要:

目的 建立胶束电动毛细管色谱二极管阵列检测法（MEKC-DAD）同时测定不同厂家的麻杏止咳糖浆中苯甲酸、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、对羟基苯甲酸丁酯等6种防腐剂的含量。方法 采用胶束电动毛细管分离模式，用未涂渍的标准熔融石英毛细管柱（75 μm×64 cm，有效长度56 cm）为分离通道；背景电解质溶液：15 mmol·L^-1硼砂-60 mmol·L^-1硼酸-50 mmol·L^-1SDS；检测波长195 nm；运行电压：15 kV；运行温度：20℃；压力进样：50 mbar，5 s。结果 各化合物的浓度与峰面积的线性关系良好（r ≥ 0.999 3）；精密度、稳定性试验的RSD<2.0%；加样回收率范围为98.7%~101.2%（n=9）。5家企业共10批样品均未检出山梨酸和对羟基苯甲酸酯类；5家企业样品的苯甲酸含量与处方相符。结论 本方法可用于麻杏止咳糖浆中防腐剂的检测，为其生产工艺和质量控制提供有意义的实验数据和参考依据。

Abstract:

OBJECTIVE To establish a micellar electrokinetic chromatography with diode array detection(MEKC-DAD) method for simultaneous determination of six preservatives including benzoic acid, sorbic acid, methylparaben, ethylparaben, propylparaben and butyl-p-hydroxybenzoate in Maxing Zhike syrup. METHODS Based on the mode of MEKC, an uncoated fused silica capillary(75 μm×64 cm, 56 cm of effective length) was adopted, and 15 mmol·L^-1borax-60 mmol·L^-1boric acid-50 mmol·L^-1SDS was selected for the running buffer. The detection wavelength was set at 195 nm. The separation voltage was 15 kV and the column temperature was maintained at 20℃. The sample was injected at 50 mbar for 5 s. RESULTS The calibration curves of the six preservatives in Maxing Zhike syrup showed good linearity(r ≥ 0.999 3). RSDs of precision and stability test were <2.0%. The average recoveries of the method were between 98.7%-101.2%(n=9). No sorbic acid and parabens were detected in 10 batches of samples from 5 enterprises. The benzoic acid content of samples from 5 enterprises was consistent with the prescription. CONCLUSION The method is suitable for the detection of preservative in Maxing Zhike syrup. The obtained results are valuable for its manufacturing process and quality control.