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刊物信息
期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
编辑部主任:粟晓黎
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237

 

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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

Tissue distribution of rutin,scutellarin and scutebarbatine B in mice after intragastric administration as determined by LC-MS/MS

分类号:
出版年·卷·期(页码):2016,36 (10):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----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,1.7 μm),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B558.4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 0~0.160 0、0.004 0~0.133 0、0.003 3~0.106 7 μg·mL-1的线性范围内线性关系良好(r≥0.991 3);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 acidacetonitrile 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·mL-1 for rutin,0.004 0-0.133 0 μg·mL-1 for scutellarin,and 0.003 3-0.106 7 μg·mL-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.

-----参考文献:---------------------------------------------------------------------------------------
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