固相萃取-高效液相色谱法测定泻痢消片中4种有效成分  

Determination of 4 kinds of effective components in Xielixiao Tablets by SPE-HPLC

作　　者：吴江瑞 齐广才[1] 崔生飞[1] 张咪咪[1] 刘珍叶[1] 

机构地区：[1]延安大学化学与化工学院,延安716000

出　　处：《西北药学杂志》2016年第4期379-383,共5页Northwest Pharmaceutical Journal

基　　金：延安大学研究生教育创新计划项目

摘　　要：目的建立采用SPE-HPLC法同时测定泻痢消片中芍药苷、甘草苷、柚皮苷和橙皮苷含量的方法。方法采用C18固相萃取柱对泻痢消片中的有效成分进行净化、富集,用HPLC法测定含量。色谱柱为Kromasil C18柱(250mm×4.6mm,5μm),流动相为乙腈-5 mL·L^(-1)磷酸溶液,梯度洗脱,检测波长为230,276和284nm,柱温为28℃,进样量为20μL,流速为1.0mL·min^(-1)。结果芍药苷、甘草苷、柚皮苷和橙皮苷分别在0.617 0~30.85(r=1.000 0),0.159 8~7.944(r=0.999 8),0.972 8~48.64(r=1.000 0)和0.123 6~6.180μg·mL^(-1)(r=0.999 9)范围内线性关系良好,平均回收率(n=6)分别为99.4%,98.3%,97.8%和97.7%。RSD值分别为0.97%,1.11%,1.28%和1.26%。结论该方法操作简单快捷,灵敏度高,结果准确,可用于泻痢消片中的4种有效成分的含量测定。Objective To establish a solid-phase extraction with high-performance liquid chromatography（SPE-HPLC）method for the determination of paeoniflorin,liquiritin,naringin,and hesperidin in Xielixiao Tablets.Methods Using C_（18） solid phase extraction column,the active ingredients of Xielixiao Tablets were purified and enriched.The contents were analyzed by HPLC method with Kromasil C_（18）column（250mm×4.6mm,5μm）.The mobile phase was composed of acetonitrile and 5mL·L^（-1） phosphoric acid in gradient elution.Detection wavelength was set at 230,276 and 284nm.The column temperature was maintained at 28℃,and injection volume was 20μL.The flow rate was 1.0mL·min^（-1）.Results The calibration curves of paeoniflorin,liquiritin,naringin,and hesperidin showed good linearity within 0.617 0-30.85（r=1.000 0）,0.159 8-7.944（r=0.999 8）,0.972 8-48.64（r=1.000 0）,and 0.123 6-6.180μg·mL^（-1）（r=0.999 9）,respectively.The average recoveries were 99.4%,98.3%,97.8% and 97.7%.RSDs were 0.97%,1.11%,1.28% and 1.26%,respectively.Conclusion The method is simple,fast,sensitive,and accurate,and can be used for the quality control of 4kinds of effective components in Xielixiao Tablets.

关 键 词：泻痢消片 芍药苷 甘草苷 柚皮苷 橙皮苷 固相萃取 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]