| UPLC-MS法测定消肿片中3个乌头碱类双酯型生物碱的含量 |
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| 引用本文： | 崔萍,杨莉,熊爱珍,王峥涛,胡春湘,詹常森.UPLC-MS法测定消肿片中3个乌头碱类双酯型生物碱的含量[J].药物分析杂志,2012(5):868-872,876. |
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| 作者姓名： | 崔萍 杨莉 熊爱珍 王峥涛 胡春湘 詹常森 |
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| 作者单位： | 中国药科大学生药学研究室;上海中医药大学中药研究所中药标准化教育部重点实验室;上海中医药大学中药研究所上海市复方中药重点实验室;上海和黄药业有限公司 |
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| 基金项目： | 上海市科学技术委员会科研计划项目(08DZ1972300);教育部“长江学者与创新团队”发展计划(IRT1071)资助 |
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| 摘 要： | 目的:建立同时测定消肿片中新乌头碱、乌头碱和次乌头碱3个双酯型生物碱含量的超高效液相色谱-质谱分析方法。方法:采用Agilent ZORBAX SB-C18(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈-0.1%甲酸水溶液(35∶65)为流动相,流速0.3 mL·min-1,柱温35℃;ESI+模式下选择离子监测(SIM)质荷比(m/z)为632,646,616的离子。结果:新乌头碱、乌头碱、次乌头碱浓度分别在0.2250～510.0 ng.mL-1(r=0.9996)、0.2500～500.0 ng.mL-1(r=0.9996)和0.2540～508.0 ng·mL-1(r=0.9996)范围内有良好的线性关系,平均回收率(n=9)分别为95.1%,93.6%,93.0%。结论:该方法简便、快捷、准确,同时检测3个有毒生物碱,可用于消肿片的质量控制。
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| 关 键 词： | 消肿片 双酯型生物碱 超高效液相色谱-质谱联用 质量控制 中成药 复方制剂 安全监测 |
Quantification of three aconitine-type diester alkaloidsin Xiaozhong tablets by UPLC-MS |
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| CUI Ping,YANG Li,XIONG Ai-zhen,WANG Zheng-tao,HU Chun-xiang,ZHAN Chang-sen.Quantification of three aconitine-type diester alkaloidsin Xiaozhong tablets by UPLC-MS[J].Chinese Journal of Pharmaceutical Analysis,2012(5):868-872,876. |
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| Authors: | CUI Ping YANG Li XIONG Ai-zhen WANG Zheng-tao HU Chun-xiang ZHAN Chang-sen |
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| Institution: | 1.Department of Pharmacognosy,China Pharmaceutical University,Nanjing 210038,China;2.The MOE Key Laboratory for Standardization of Chinese Medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;3.Shanghai Key Laboratory for Compound Chinese Medicines, Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China; 4.Shanghai Hutchison Pharmaceuticals,Shanghai 200331,China) |
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| Abstract: | Objective:To establish an UPLC-MS method for simultaneous quantification of mesaconitine,aconitine and hypaconitine in Xiaozhong tablets.Methods:The separation was performed on an Agilent ZORBAX SB-C18(100 mm×2.1 mm,1.8 μm)column with acetonitrile-0.1% formic acid(35∶65)as the mobile phase.The column temperature was set at 35 ℃ with flow rate of 0.3 mL·min-1.AP-ESI at positive ion mode and the selected ion monitoring were used.Ions at m/z 632,646 and 616 were selected to quantify mesaconitine,aconitine and hypaconitine.Results:The linear ranges were 0.2250-510.0 ng·mL-1(r=0.9996)for mesaconitine,0.2500-500.0 ng·mL-1(r=0.9996)for aconitine and 0.2540-508.0 ng·mL-1(r=0.9996)for hypaconitine.The average recoveries(n=9)were 95.1% for mesaconitine,93.6% for aconitine and 93.0% for hypaconitine.Conclusion:The established method is convenient,rapid and accurate,which can be used to determine three poisonous alkaloids in Xiaozhong tablets.The study may provide a scientific basis for the quality control of this preparation. |
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| Keywords: | Xiaozhong tablets diester-diterpenoid alkaloids UPLC-MS quanlity contral Chinese patent medicine compound preparation safety monitoring |
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