亲水作用毛细管电色谱分析苷类药物的研究
Analysis of glycosides by hydrophilic interaction capillary electrochromatographyelectrochromatography

基于多面体寡聚硅倍半氧烷-甲基丙烯酸羟乙酯poly(POSS-MA-co-HEMA)有机硅胶杂化整体柱，建立典型苷类药物（连翘苷、豆腐果苷、紫丁香苷、天麻素）的亲水作用毛细管电色谱检测技术. 考察流动相乙腈比例、缓冲液浓度、缓冲溶液pH值、分离电压和反压阀压力对四种苷类药物分离效果的影响，在最优条件下（流动相为2 mmol·L-1磷酸三乙胺缓冲液（乙腈体积分数为90%，pH=7.0），分离电压-8 kV、柱压力5.4 MPa），4种苷类药物在10 min内得到了基线分离. 连翘苷、豆腐果苷、紫丁香苷和天麻素线性范围分别为10~200、25~200、15~200 和25~200 μg·mL-1，检测限为1.5~8.0 μg·mL-1. 应用于血清模拟样品分析，平均回收率为95.6%~99.1%，相对标准偏差小于3.3%. A
hydrophilic interaction capillary electrochromatography with silica-hybrid monolithic column has been developed for the separation and determination of four glycosides (including forsythin，helicid，syringin and gastrodin). The effect factors such as organic modifier，acidity and concentration of running buffer，separation voltage and supplement pressure were investigated to acquire the optimum condition. Under the optimal conditions，four glycosides could be baseline-separated rapidly within 10 min with the separation voltage of -8 kV in 2 mmol·L-1 triethylamine phosphate buffer (pH=7.0) containing 90% acetonitrile and supplement pressure of 5.4 MPa. The calibration graphs of forsythin，helicid，syringin and gastrodin were linear by plotting the peak area against the analytes concentration over the range of 10~200，25~200，15~200 and 25~200 μg·mL-1，respectively. The detection limits of four glycosides were ranged from 1.5 to 8.0 μg·mL-1 and the recoveries of serum samples were about 95.6%~99.1% ，RSD≤3.3%