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液质联用分析芦丁、野黄芩苷和半枝莲碱B在小鼠灌胃给药后体内的组织分布
  • ISSN号:0254-1793
  • 期刊名称:《药物分析杂志》
  • 时间:0
  • 分类:R917[医药卫生—药物分析学;医药卫生—药学]
  • 作者机构:[1]南京中医药大学转化医学研究中心国家中医药管理局名医验方评价与转化重点研究室江苏省抗肿瘤验方研究与产业化工程实验室,南京210023, [2]南京中医药大学药学院,南京210023, [3]江苏省中医药防治肿瘤协同创新中心,南京210023
  • 相关基金:国家自然科学基金项目(NO.81373511,81573910);国家自然科学基金青年项目(81403079);江苏省自然科学基金项目(BK20141467)
中文摘要:

目的:建立UPLC-MS同时测定小鼠组织中芦丁、野黄芩苷和半枝莲碱B的分析方法,并对该3种成分在小鼠体内的组织分布进行研究。方法:以2-氰基-3,12-二氧代齐墩果烷-1,9(11)-二烯-28-酸甲酯(CDDO-Me)为内标,通过甲醇沉淀组织样品蛋白,使用LC-MS技术进行定量分析,采用ACQUITY UPLC BEH-C18色谱柱(100 mm×2.1 mm,1.7μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,正、负离子检测模式,检测离子质荷比(m/z)为芦丁609.2、野黄芩苷463.3、半枝莲碱B 558.4和CDDO-Me 506.7。结果:在小鼠肝脏、心脏、脾脏、肺脏、肾脏等组织中,芦丁、野黄芩苷、半枝莲碱B分别在0.005 00.160 0、0.004 00.133 0、0.00330.106 7μg·m L-1的线性范围内线性关系良好(r≥0.9913);方法的精密度和稳定性RSD均小于15%;回收率为90.0%98.4%,RSD小于15%,符合化学药物非临床药代动力学研究技术指导原则。芦丁等3个成分在小鼠体内分布比较广泛,其中在肝脏和肾脏中分布较多,在肺脏中分布含量最低。结论:本方法经方法学验证,可对小鼠组织中的芦丁、野黄芩苷、半枝莲碱B含量进行测定;在用于小鼠体内化学成分的组织分布研究中,芦丁在肾脏中含量多、脾脏中最少,野黄芩苷在心脏中含量最多、肺脏中最少,半枝莲碱B在肝脏中含量最多、肾脏中最少。

英文摘要:

Objective:To establish a UPLC-MS method for simultaneous determination of rutin,scutellarin and scutebarbatine B in mice tissues and apply the method to tissue distribution study of these three components.Methods:The tissue samples were precipitated with methanol and analyzed by LC-MS with 0.1% formic acid-acetonitrile solution as the gradient elution mobile phase.The separation was performed on an ACQUTITY UPLC BEH-C18(100 mm×2.1 mm,1.7 μm),and 2-cyano-3,12-dioxo Oleanane-1,9(11)-28- diene acid methyl ester(CDDO-Me)was used as an internal standard.The mass spectrometer was operated in positive and negative electrospray ionization modes,and the transition m/z 609.2,m/z 463.3,m/z 558.4 and m/z 506.7 were used for rutin,scutellarin,scutebarbatine B and CDDO-Me,respectively.Results:Excellent linearity(r ≥0.991 3)was observed in all three studied components within their linear ranges,with 0.005 0-0.160 0 μg·m L-1 for rutin,0.004 0-0.133 0 μg·m L-1 for scutellarin,and 0.003 3-0.106 7 μg·m L-1 for scutebarbatine B.The RSD of precision and stability of the developed method was less than 15%.The recovery of the method was 90.0%-98.4% with RSD less than 15%,in line with the technical guidelines for non-clinical pharmacokinetic study of chemical drugs.Rutin,scutellarin and scutebarbatine B were widely distributed in mice tissues.The majority was detected in liver and kidney,and the lowest content was in lung.Conclusion:The method is proved by methodological validation that it can be used for content determination of rutin,scutellarin and scutebarbatine B in mice tissues.Rutin was detected mostly in kidney and the lowest was found in spleed,scutellarin was detected mostly in heart and the lowest was found in lung,and scutebarbatine B was detected mostly in liver and the lowest was found in kidney.

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期刊信息
  • 《药物分析杂志》
  • 中国科技核心期刊
  • 主管单位:中国科协
  • 主办单位:中国药学会
  • 主编:金少鸿
  • 地址:北京天坛西里2号
  • 邮编:100050
  • 邮箱:ywfx@nifdc.org.cn
  • 电话:010-67058427
  • 国际标准刊号:ISSN:0254-1793
  • 国内统一刊号:ISSN:11-2224/R
  • 邮发代号:2-237
  • 获奖情况:
  • 四通杯全优期刊奖,92、97年获科协优秀期刊三等奖,96年影响因子全年第一
  • 国内外数据库收录:
  • 美国国际药学文摘,美国化学文摘(网络版),日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:32603