MEKC法同时测定小儿止咳糖浆中6种防腐剂的含量

Simultaneous Determination of Six Preservatives in Pediatric Cough Syrup by MEKC

目的:建立胶束高效毛细管电泳(MEKC)同时测定小儿止咳糖浆中苯甲酸、山梨酸、羟苯甲酯、羟苯乙酯、羟苯丙酯、羟苯丁酯的方法。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(75μm×50 cm,42 cm)为分离通道;分离缓冲液为15 mmol·L^-1Na2B4O7-H3BO-3溶液(p H 8.7,含50 mmol·L^-1SDS);检测波长195 nm;运行电压:15 k V;柱温度:25℃;压力进样:50 mbar,5s。结果:6种防腐剂在各自浓度的范围内线性关系良好(r=0.9993~0.9998),平均加样回收率在97.1%~102.2%范围内,RSD均小于2.0%(n=9)。11家企业共22批样品中苯甲酸的含量均符合规定,其余5种防腐剂未检出。结论:本方法专属性强,准确度高,重复性良好,可用于小儿止咳糖浆中防腐剂的检测,为其生产工艺和质量控制提供参考依据。

Objective:To establish a method for the simultaneous determination of benzoic acid,sorbic acid and methyl,ethyl,propyl and butyl p-hydroxybenzoates in pediatric cough syrup by micellar electrokinetic chromatography(MEKC).Methods:Based on the mode of MEKC,an uncoated fused silica capillary(75μm×50 cm,42 cm)column was adopted,and 15 mmol·L^-1 Na2B4O7-H3BO3(p H8.7,Containing 50 mmol·L^-1 SDS)was selected as the running buffer.The detection wavelength was set at 195 nm.The separation voltage was 15 k V and the column temperature was maintained at 25℃.The sample was injected at 50 mbar for 5 s.Results:The calibration curves of the six preservatives in pediatric cough syrup showed good linearity(r=0.9993-0.9998).The average recoveries of the method were between 97.1%and 102.2%(RSD<2.0%,n=9).The content of benzoic acid in 22 batches of samples from 11 enterprises met the requirements,and the remaining 5 preservatives were not detected.Conclusion:The method is good in resolution,sensitivity and reproducibility.It can be used for the detection of preservatives in pediatric cough syrup,which provides reference for the control of the production process and the quality of the preparation.