摘要
目的：建立一种快速准确的同时测定当归芍药散中阿魏酸和芍药苷的方法。方法：采用超高效液相色谱．串联质谱检测技术，分别以羟甲香豆素和栀子苷为内标，采用正离子方式检测，MRM模式扫描，检测离子通道为阿魏酸m／z195．1-151．2和羟甲香豆素m／z177．1—161，2、芍药苷m／z503，1-219．2和栀子苷m／z411．1-216．1；色谱柱为WatersC。ACQU／TYUPLCBEH（2．1mm-150ram，1．7μm），流动相为0．5％冰醋酸．乙腈（82：18，v／v）。结果：四个成分3rain内完成检测；阿魏酸的线性范围为4．50ng·m-1～250．0ng·mL-1，定量限为0．25ng·mL-1，芍药苷的线性范围为37．50ng·mL～2000．0ng·mL-1，定量限为37．50ng·mL-1；平均加样回收率分别为101．2士1．7％，99．8士1．6％和99．7士1．5％（阿魏酸），99．5士1．6％、100．21．4％和100．7士1．2％（芍药苷）；保留时间分剐为栀子苷1．1min、芍药苷1．3min、羟甲香豆素2．1min，阿魏酸2．9min。结论：该方法分析时间短、专属性好、准确度高，适用于同时测定当归芍药散中的阿魏酸和芍药苷。
Objective： To establish a fast and accurate method to Simultaneous determine Ferulic acid and Paeoniflorin in Dangguishaoyao San. Meth- otis： Using Hymecromone and Geniposide as the internal, the application of the technology of ultra performance liquid chromatography - tandem mass spectrometry have been done by using the positive ion mode detection, MRM mode scan and detect ion channels rrdz195.1---}151.2 for Ferulic acid, mJz177.1---}161.2 for Hymecromone, m/z503.1--}219.2 for Paeoniflorin and m/z411.1--216.1 for Geniposide, the separation was performed a Waters C, ACQUITY UPLC BEH （2.1ram 150nu, 1.7m）column with the mobile phase of 0.5%glacial acetic acid-acetonitrile （82：18, v/v）. Re- sults： Four components were determined within 3 min. The linear range of Ferulic acid is 4.50rig . mL-250.0ng.mL-1, limit of quantification is 4.50rig. mL＂, and the linear range of Paeoniflorin is 37.50ng .mL--2000.0ng. mL-1, limit of quantification is 37.50 rig＇ mL＂, the average recoveries are 101.2.7%, 99.8士1.6%, 99.7士1.5% （Ferulic acid） and 99.5士1.6%, 100.2士1.4%, 100.7士1.2% （Paeoniflorin）. The retention time of Ferulic acid,Hymecromone, Paeoniflorin and Geniposide are 1.1min, 1.3min, 2.1min and 2.9rain respectively. Conclusion： The analysis time of the method is short and the method has high specificity, accuracy, can be used for simultaneous determination of Ferulic acid and Paeoniflorin in Dangguishaoyao San.
出处
《按摩与康复医学》
2013年第7期147-150,共4页
Chinese Manipulation and Rehabilitation Medicine
