| 摘要: |
| 目的建立扶正平消胶囊中4种成分含量的高效液相色谱-质谱(HPLC-MS)测定方法。方法色谱条件:Agilent Eclipse plus C18色谱柱(250 mm×4.6 mm,5 μm)；乙腈(A)-0.1%甲酸水(B)为流动相,梯度洗脱程序为0 min(AB=1585); 30 min(AB=4060)。质谱条件:采用电喷雾离子源(ESI)，负离子电离,选择性离子监测(SIM)模式。结果龙胆苦苷、甘草苷、迷迭香酸和哈巴俄苷的定量限分别为5.73、6.37、6.50和6.46 ng/ml,检测限分别为0.46、0.32、0.33和0.32 ng/ml；在相应的线性范围内,r>0.999 0；待测物与内标的峰面积之比的日内精密度和日间精密度均小于2%,平均回收率为98%~102%。结论所建立的HPLC-MS方法可同时测定扶正平消胶囊中龙胆苦苷、甘草苷、迷迭香酸和哈巴俄苷的含量,快速、简便,实用性强。 |
| 关键词: 扶正平消胶囊 龙胆苦苷 甘草苷 迷迭香酸 哈巴俄苷 HPLC-MS |
| DOI：10.3724/SP.J.1008.2011.0524 |
| 投稿时间：2010-12-29修订日期：2011-03-09 |
| 基金项目: |
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| HPLC-MS in simultaneous determination of 4 compounds in Fuzhengpingxiao capsule: gentiopicroside, liquiritin, rosmarinic acid and harpagoside |
| TIAN Wen-jun1,JIA Jing1,ZHAO Liang1,L Lei1,LI Yue-yue1,ZHANG Hai1,ZHANG Guo-qing1* |
| (1. Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China; 2. Department of Pharmacy, No.175 Hospital of PLA, Southeast Hospital Affiliated to Xiamen University, Zhangzhou 363000, Fujian, China) |
| Abstract: |
| ObjectiveTo establish a HPLC-MS method to simultaneously determine the contents of gentiopicroside, liquiritin, rosmarinic acid and harpagoside in Fuzhengpingxiao capsule. MethodsThe chromatographic separation was performed on a Agilent Eclipse plus C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase of acetonitrile(A)-0.1% methanoic acid(B) (0-30 min, 15%A-40%A), eluted at a flow rate of 1.0 ml/min and with a split ratio of 31. Negative ionization and selected ion monitoring(SIM) mode on Mass were selected. ResultsThe limit of quantitation(LOQ) values of gentiopicroside, liquiritin, rosmarinic acid and harpagoside were 5.73, 6.37, 6.50, and 6.46 ng/ml, and the limit of detection(LOD) values were 0.46, 0.32, 0.33 and 0.32 ng/ml, respectively. Good linearity (r>0.999 0) was obtained over the investigated concentration ranges. Reproducibility was evaluated by intra- and inter-day assays, and RSD values were below 2%. The average recoveries of the 4 compounds were within the range of 98%-102%. ConclusionWe have established a rapid and efficient HPLC-MS method for determination of 4 constituents in Fuzhengpingxiao capsule: gentiopicroside, liquiritin, rosmarinic acid and harpagoside. |
| Key words: Fuzhengpingxiao capsule gentiopicroside liquiritin rosmarinic acid harpagoside |
