HPLC-MS/MS法测定不同采收期连翘叶中9种成分  

Determination of nine components in Forsythia Folium collected in different periods

作　　者：支旭然[1] 苑霖[1] 生宁[1] 张志勇[1] 张晓旭[1] 贾佩佩[1] 张兰桐[1] 

机构地区：[1]河北医科大学药学院药物分析教研室,河北石家庄050017

出　　处：《中草药》2013年第22期3231-3235,共5页Chinese Traditional and Herbal Drugs

基　　金：河北省自然科学基金-石药集团医药联合研究基金(优先资助项目)(H2012206079)

摘　　要：目的建立HPLC-MS/MS法同时测定连翘叶中连翘苷、连翘脂素、连翘酯苷A、连翘酯苷F、芦丁、槲皮素、异槲皮苷、绿原酸、(+)-表松脂素-4′-O-葡萄糖苷的量。方法采用Dikma Diamonsil C18色谱柱(150 mm×4.6 mm,5μm),柱温30℃,以甲醇-0.02%甲酸水溶液为流动相进行梯度洗脱,体积流量0.8 mL/min,进样量10μL;采用电喷雾离子源进行负离子模式监测,多反应监测模式(MRM)用于定量分析,源喷射电压为4 500 V,离子源温度为650℃。结果 9种化学成分的峰面积和浓度在测定浓度范围内均具有良好的线性关系,加样回收率为97.20%～101.2%,精密度RSD为0.54%～1.24%。结论本法简便快速、灵敏度高、专属性好,可用于连翘叶中9种活性成分的测定。通过对结果进行分析,连翘叶以5月份采收最佳。Objective To develop an HPLC-MS method for the determination ofphillyrin, phillygenin, forsythiaside A, forsythiaside F, rutin, quercetin, isoquercitrin, chtorogenic acid, and （＋）-epipinoresinol-4＇-O-glucoside in Forsythia Folium. Methods The samples were separated on a Dikma Diamonsil C18 column （150 mm × 4.6 mm, 5 μm）, eluted with methanol and water containing 0.02% formic acid in a gradient elution at a flow rate of 0.8 mL/min, and the injection volume was 10 μL. The column temperature was set at 30 ℃. The multiple-reaction monitoring scanning was employed for the quantification with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at -4 500 V and the turbo spray temperature was maintained at 650 ℃. Results The regression equations showing linear relationships between peak areas and contents of each compound were obtained. The average recoveries of the compounds ranged from 97.20% to 101.2% and the precision in terms of RSD was in the range of 0.54%--1.24%. Conclusion The method is sensitive and suitable for the determination of the nine components in Forsythia Folium. As a result, the suitable harvesting time for Forsythia Folium is May.

关 键 词：连翘叶 HPLC-MS 连翘苷 连翘酯苷 连翘脂素 

分 类 号：R286.02[医药卫生—中药学]