超高效液相色谱-串联质谱双内标法同时测定复方杏香兔耳风胶囊中的10种有效成分  

Simultaneous determination of ten constituents in the Chinese medicinal preparation Fufangxingxiangtu ' erfengcapsules byultra performance liquid chromatographywith tandem mass spectrometry

作　　者：范晓苏[1,2] 庞倩[2] 徐远金[1,2] 

机构地区：[1]亚热带农业生物资源保护与利用国家重点实验室,广西大学,广西南宁530004 [2]广西大学化学化工学院,广西南宁530004

出　　处：《色谱》2014年第3期216-223,共8页Chinese Journal of Chromatography

基　　金：广西自然科学基金项目(桂科自0832034)

摘　　要：建立了同时测定复方杏香兔耳风胶囊中原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III 和白术内酯 I 等10种有效成分含量的超高效液相色谱-串联质谱（ UPLC-MS / MS）双内标分析方法。以咖啡酸和淫羊藿苷为内标（IS），在 ZORBAX RRHD Eclipse Plus C 18色谱柱上，以甲醇和含0.3％甲酸的水为流动相进行梯度洗脱分离，流速为0.3 mL / min。在电喷雾电离（ESI）正、负离子切换模式下，采用多重反应监测模式进行检测。结果表明，原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III、白术内酯 I 的线性范围分别为0.00300～24.0 mg / L、0.0170～2.00 mg / L、0.0150～30.0 mg / L、0.00400～30.0 mg / L、0.0105～24.0 mg / L、0.00300～30.0 mg / L、0.00300～5.00 mg / L、0.00600～5.00 mg / L、0.00150～4.00 mg / L、0.000600～0.900 mg / L；检出限分别为1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20μg / L。10种成分的加样回收率为92.5％～106％，相对标准偏差均不大于3.2％。该方法快速简便、灵敏度高、重复性好，已成功用于实际样品的分析。Using caffeic acid and icariin as internal standards,a method for the simultaneous determination of protocatechuic acid,protocatechuic aldehyde,chlorogenic acid,scutellarin, isochlorogenic acid C,baicalin,luteolin,apigenin,atractylenolide III and atractylenolide I in Fufangxingxiangtu’erfeng capsules were established by ultra performance liquid chromatogra-phy with tandem mass spectrometry（UPLC-MS / MS）. The separation was performed on a ZOR-BAX RRHD Eclipse Plus C 18 column（ 50 mm ＆#215; 2. 1 mm,1. 8 μm）by using water containing 0. 3% formic acid and methanol as mobile phases with the gradient elution at a flow rate of 0. 3 mL / min. The analytes were detected by a tandem mass spectrometer in the multiple reaction monitoring（MRM）mode via the switching of positive electrospray ionization（ESI ＋）and nega-tive electrospray ionization（ESI -）. Under optimum conditions,the calibration curves were lin-ear in the range of 0. 003 00-24. 0 mg / L for protocatechuic acid,0. 017 0-2. 00 mg / L for proto-catechuic aldehyde,0. 015 0-30. 0 mg / L for chlorogenic acid,0. 004 00-30. 0 mg / L for scutella-rin,0. 010 5-24. 0 mg / L for isochlorogenic acid C,0. 003 00-30. 0 mg / L for baicalin,0. 003 00-5. 0 mg / L for luteolin,0. 006 00-1. 50 mg / L for apigenin,0. 001 50-4. 00 mg / L for atractylenol-ide III,and 0. 000 600 - 0. 900 mg / L for atractylenolide I with the detection limits of 1. 0,11, 5. 0,1. 5,3. 5,1. 0,1. 0,2. 0,0. 50,0. 20 μg / L,respectively. The average recoveries of the ten effective components were between 92. 5% and 106% with all relative standard deviations not more than 3. 2% . The developed method was rapid,simple,accurate,reproducible,and suit-able for the quality control of the Fufangxingxiangtu’erfeng capsules.

关 键 词：超高效液相色谱-串联质谱 有效成分 复方杏香兔耳风胶囊 ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS MS) 

分 类 号：O658[理学—分析化学]