UPLC-MS/MS法同时测定经典名方实脾散中20个化学成分的含量  

Simultaneous determination of twenty chemical components in Shipi powder by UPLC-MS/MS

作　　者：麻景梅[1] 姜晓娅 麻朝朝 李琛[1] 范帅帅[1] 王鑫国[1] 牛丽颖[1] MA Jing-mei;JANG Xiao-ya;MA Zhao-zhao;LI Chen;FAN Shuai-shuai;WANG Xin-guo;NIU Li-ying(Hebei University of Traditional Chinese Medicine,Hebei Traditional Chinese Medicine Formula Granule Engineering&Technology Innovate Center,Quality Evaluation&Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine,Shijiazhuang 050091,China;Guizhou University of Traditional Chinese Medicine,Guiyang 550025,China)

机构地区：[1]河北中医学院,河北省中药配方颗粒技术创新中心,中药材品质评价与标准化河北省工程研究中心,石家庄050091 [2]贵州中医药大学,贵阳550025

出　　处：《药物分析杂志》2023年第3期429-439,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：中央引导地方科技发展资金项目(206Z2501G);河北省重点研发计划项目(20372502D);河北省自然科学基金资助项目(H2019423050)。

摘　　要：目的:建立UPLC-MS/MS法同时测定实脾散中20个化学成分(槟榔碱、环磷酸腺苷、新绿原酸、绿原酸、隐绿原酸、咖啡酸、甘草苷、苯甲酰新乌头原碱、苯甲酰乌头原碱、异甘草苷、苯甲酰次乌头原碱、甘草素、异甘草素、甘草酸、6-姜辣素、和厚朴酚、木香烃内酯、去氢木香内酯、厚朴酚、白桦脂酸)的含量。方法:采用岛津Shim-pack GIST C18色谱柱(100 mm×2.1 mm, 2μm),流动相为0.1%甲酸水(A)-乙腈(B),梯度洗脱(0~12 min, 2%B→14%B;12~24 min, 14%B→51%B;24~26 min, 51%B→70%B;26~36 min, 70%B;36~37 min, 70%B→2%B;37~40 min, 2%B),柱温为35℃,流速为0.3 mL·min^(-1),进样量为1μL;采用电喷雾电离源(ESI源),多重反应监测(MRM)模式正负离子检测。结果:20个化学成分在测定浓度范围内线性关系良好,相关系数均>0.997 6;精密度、重复性和稳定性良好;平均加样回收率为93.4%~108.7%,RSD≤5.0%。15批样品中槟榔碱、环磷酸腺苷、新绿原酸、绿原酸、隐绿原酸、咖啡酸、甘草苷、苯甲酰新乌头原碱、苯甲酰乌头原碱、异甘草苷、苯甲酰次乌头原碱、甘草素、异甘草素、甘草酸、6-姜辣素、和厚朴酚、木香烃内酯、去氢木香内酯、厚朴酚、白桦脂酸测定结果分别为7 190.26~13 726.74、90.11~301.93、9.65~71.13、102.88~710.98、40.51~179.73、10.90~71.22、3 424.43~27 337.63、508.34~1 276.14、108.27~192.65、95.74~378.92、565.19~1 018.53、106.23~623.42、3.53~16.47、6 104.50~15 933.93、1 047.58~1 750.15、537.91~2 582.74、332.83~581.28、348.22~760.81、350.65~2 189.73、2.06~39.22μg·g-1。结论:本方法准确灵敏,稳定性和重复性好,可用于实脾散的质量控制。Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of twenty chemical components(arecoline hydrobro-mide,adenosine cyclophosphate,neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,caffeic acid,liquiritin,benzoylmesaconine,benzoylaconitine,isoliquiritin,benzoylhypacoitine,liquiritigenin,isoliquiritige-nin,glycyrrhizic acid,6-gingerol,honokiol,costunolide,dehydrocostus lactone,magnolol,betulinic acid)in Shipi powder.Methods:The separation was performed over 40.0 min on a Shim-pack GIST C18 column(100 mm×2.1 mm,2.0μm)with a mobile phase consisting of 0.1%formic acid in water and acetonitrile with gradi-ent elution(0-12 min,2%B→14%B;12-24 min,14%B→51%B;24-26 min,51%B→70%B;26-36 min,70%B;36-37 min,70%B→2%B;37-40 min,2%B)at a flow rate of 0.3 mL·min^(-1).The column tempera-ture was 35℃and the injection volume was 1μL.The detection was carried out by electrospray ionization(ESI).Positive and negative electrospray ionizations were performed in multiple reaction monitoring(MRM)mode.Results:All of the analytes showed good linearity(r≥0.9976)in the tested ranges.The precision,repeatability and stability of the method were good for the twenty chemical components.The average recoveries were in the range of 93.4%-108.7%with relative standard deviations RSD≤5.0%.The contents of arecoline,adenosine cyclophosphate,neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,caffeic acid,liquiritin,benzoylmesaconine,benzoylaconitine,isoliquiritin,benzoylhypacoitine,liquiritigenin,isoliquiritigenin,glycyr-rhizic acid,6-gingerol,honokiol,costunolide,dehydrocostus lactone,magnolol,betulinic acid in 15 bantches of in Shipi powder were 7190.26-13726.74,90.11-301.93,9.65-71.13,102.88-710.98,40.51-179.73,10.90-71.22,3424.43-27337.63,508.34-1276.14,108.27-192.65,95.74-378.92,565.19-1018.53,106.23-623.42,3.53-16.47,6104.50-15933.93,1047.58-1750.15,537.91-2582.74,332.83-581.28,348.22-760.81,350.65-2189.73,2.06-39.22μ

关 键 词：经典名方 实脾散 液相色谱-质谱联用 多重反应监测 化学成分 含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学]