MEKC法同时测定中药口服液体制剂中10种防腐剂和甜味剂含量

Simultaneous Determination of 10 preservatives and Sweeteners in oral liquid preparation of traditional Chinese medicine by MEKC

关键词:  胶束电动毛细管色谱  中药口服液体制剂  防腐剂  甜味剂  苯甲酸钠  羟苯乙酯  含量测定

Key words:  micellar electrokinetic chromatography(MEKC)  oral liquid preparation of traditional Chinese medicine  preservatives  sweeteners  sodium benzoate  ethyl paraben  content determination

摘要:

目的 建立胶束电动毛细管色谱法(micellar electrokinetic chromatography，MEKC)同时测定6种中药口服液体制剂中的10种添加剂。方法 以40%乙腈水溶液作为提取溶剂，经涡旋混匀、高速离心过滤后进行MEKC分析。采用未涂渍的标准熔融石英毛细管柱(75 μm×68.5 cm，有效长度60 cm)作为分离通道，以50 mmol·L^-1硼酸盐缓冲液(pH 8.4，含20 mmol·L^–1十二烷基硫酸钠)为运行缓冲液，分离电压20 kV，柱温25 ℃，检测波长为200 nm。结果 10种待测物在相应的质量浓度范围内线性关系良好，相关系数(r)为0.996 9~0.999 7；检出限为0.05~0.15 μg·mL^–1，定量限为0.16~0.50 μg·mL^–1，平均回收率为84.3%~100.6%(RSD为1.1%~5.1%)。样品测定结果显示，30个中药口服液体制剂检出苯甲酸钠和羟苯乙酯，其余未检出。苯甲酸的检出率为100%，含量为0.09%~0.3%。羟苯乙酯的检出率为33%，含量为0.03%~0.05%。结论 该方法样品前处理简单，具有专属性好、准确、高效等优点，可用于中药口服液体制剂中10种添加剂成分的含量测定。

Abstract:

OBJECTIVE To develope a micellar electrokinetic chromatography(MEKC) method for the simultaneous determination of ten possible additives in 6 oral liquid preparations of traditional Chinese medicine. METHODS The samples were extracted with 40% acetonitrile aqueous solution, followed by vortex mixing, high-speed centrifugation and finally analyzed by MEKC. The chromatographic separation was performed on an uncoated fused-silica capillary column(75 μm×68.5 cm, effective length 60 cm) with 50 mmol·L^-1 borax buffer(pH 8.4, containing 20 mmol·L^-1 SDS). The separation voltage was 20 kV, and the column temperature was maintained at 25℃. The detection wavelength was set at 200 nm. RESULTS The 10 analytes showed good linearity within their respective concentration ranges, with correlations coefficients(r) of 0.996 9-0.999 7. The limits of detection(LOD) and limits to quantitation(LOQ) of the method were in the ranges of 0.05-0.15 μg·mL^-1 and 0.16-0.50 μg·mL^-1, respectively. The average recoveries ranged from 84.3% to 100.6%, with RSDs of 1.1%-5.1%. The detection results showed that sodium benzoate and ethyl paraben were detected in 30 oral liquid preparations of traditional Chinese medicine, while others were not detected. The detection rate of sodium benzoate was 100%, and the content was 0.09%-0.3%. The detection rate of ethyl paraben was 33%, and the content was 0.03%-0.05%. CONCLUSION The method has the advangtages of simple sample pretreatment, good specificity, accuracy, and high efficiency, and can be used for the determination of 10 additives in oral liquid preparations of traditional Chinese medicine.