CAJ | 학술논문

　　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Waters C18 ACQUITY UPLC BEH （2.1 mm×150mm，1.7μm），流动相为0.5%冰醋酸-乙腈（82：18，v/v）。结果：四个成分3min内完成检测；阿魏酸的线性范围为4.50ng·mL-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-1~2000.0ng·mL-1，定量限为37.50ng·mL-1；平均加样回收率分别为101.2±1.7%、99.8±1.6%和99.7±1.5%（阿魏酸），99.5±1.6%、100.2±1.4%和100.7±1.2%（芍药苷）；保留时间分别为栀子苷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。
　　목적：건립일충쾌속준학적동시측정당귀작약산중아위산화작약감적방법。방법：채용초고효액상색보-천련질보검측기술，분별이간갑향두소화치자감위내표，채용정리자방식검측，MRM모식소묘，검측리자통도위아위산m/z195.1→151.2화간갑향두소m/z177.1→161.2、작약감m/z503.1→219.2화치자감m/z411.1→216.1；색보주위Waters C18 ACQUITY UPLC BEH （2.1 mm×150mm，1.7μm），류동상위0.5%빙작산-을정（82：18，v/v）。결과：사개성분3min내완성검측；아위산적선성범위위4.50ng·mL-1~250.0ng·mL-1，정량한위0.25ng·mL-1，작약감적선성범위위37.50ng·mL-1~2000.0ng·mL-1，정량한위37.50ng·mL-1；평균가양회수솔분별위101.2±1.7%、99.8±1.6%화99.7±1.5%（아위산），99.5±1.6%、100.2±1.4%화100.7±1.2%（작약감）；보류시간분별위치자감1.1min、작약감1.3min、간갑향두소2.1min，아위산2.9min。결론：해방법분석시간단、전속성호、준학도고，괄용우동시측정당귀작약산중적아위산화작약감。
Objective:To establish a fast and accurate method to Simultaneous determine Ferulic acid and Paeoniflorin in Dangguishaoyao San. Meth-ods: 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 m/z195.1→151.2 for Ferulic acid, m/z177.1→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 C18 ACQUITY UPLC BEH (2.1mm × 150mm, 1.7μm)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 4.50ng·mL-1~250.0ng·mL-1, limit of quantification is 4.50ng·mL-1, and the linear range of Paeoniflorin is 37.50ng·mL-1~2000.0ng·mL-1, limit of quantification is 37.50 ng·mL-1, the average recoveries are 101.2±1.7%, 99.8±1.6%, 99.7±1.5%(Ferulic acid) and 99.5±1.6%, 100.2±1.4%, 100.7±1.2%( Paeoniflorin). The retention time of Ferulic acid,Hymecromone, Paeoniflorin and Geniposide are 1.1min, 1.3min, 2.1min and 2.9min 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.