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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
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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UHPLC-MS/MS技术同时测定大鼠灌胃白花蛇舌草水提取液后血浆中3种二萜类成分含量及其药代动力学研究

Simultaneous determination of three iridoids in rat plasma after oral administration of Oldenlandia diffusa(Willd.)water extract by UHPLC-MS/MS

作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (5):813-820
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立超高效液相色谱-质谱联用(UHPLC-MS/MS)方法,同时测定大鼠灌胃白花蛇舌草水提取物后血浆中去乙酰车叶草苷酸、去乙酰车叶草苷酸甲酯和京尼平苷酸的含量。方法:使用C18色谱柱(100 mm×2.1 mm,1.8 μm),以乙腈-0.1%甲酸水为流动相梯度洗脱,流速为0.3 mL·min-1;采用质谱检测法,多反应监测(MRM)方式检测。结果:各成分线性良好,r2均≥ 0.993 4。各成分日内及日间精密度均在15%以内,准确度回收率范围为91.8%~99.0%。血浆中各待测物及内参提取回收率均≥ 94.5%。去乙酰车叶草苷酸、去乙酰车叶草苷酸甲酯及京尼平苷酸分别在灌胃后0.5、3和3 h达到最高浓度,AUC(0-t分别为(1 281.95±1 079.75)、(1 679.10±681.93)、(129.35±69.23)ng·L-1·h-1,AUC(0-∞)分别为(1 373.21±1 054.31)、(2 018.92±1 102.21)、(152.94±71.34)ng·L-1·h-1t1/2分别为(6.50±5.95)、(8.54±4.14)、(5.22±2.11)h,MRT(0-t分别为(6.08±0.86)、(7.98±2.59)、(8.31±3.35)h。结论:该UHPLC-MS/MS方法成功地应用于大鼠灌胃白花蛇舌草提取物后的3种二萜类成分药物代谢动力学研究。

-----英文摘要:---------------------------------------------------------------------------------------

Objective:To develop and validate a rapid and sensitive ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for the simultaneous determination of deacetylasperulosidic acid, deacetylasperulosidic acid methyl ester and geniposidic acid in rat plasma after oral administration of Oldenlandia diffusa (Willd.) water extract.Methods:The analytes were separated on a C18 column (100 mm×2.1 mm, 1.8 μm) with acetonitrile-0.1% aqueous formic acid solution as the mobile phase.The flow rate was set at 0.3 mL·min-1.The analytes were monitored by mass spectrometry with multiple reaction monitoring (MRM).Results:The linearity r2 was ≥ 0.993 4 for all the analytes.The intra-and inter-day precision were all within 15%, and the accuracies ranged from 91.8% to 99.0%.The mean extraction recoveries of analytes and IS from rat plasma were all ≥ 94.46%.Deacetylasperulosidic acid, deacetylasperulosidic acid methyl ester and geniposidic acid ester reached highest concentrations at 0.5, 3 and 3 h after oral administration.The pharmacokinetic of deacetylasperulosidic acid, deacetylasperulosidic acid methyl ester and geniposidic acid ester were AUC(0-t):(1 281.95±1 079.75) ng·L-1·h-1, (1 679.10±681.93) ng·L-1·h-1, (129.35±69.23) ng·L-1·h-1, AUC(0-∞):(1 373.21±1 054.31) ng·L-1·h-1, (2 018.92±1 102.21) ng·L-1·h-1, (152.94±71.34) ng·L-1·h-1, t1/2:(6.50±5.95) h, (8.54±4.14) h, (5.22±2.11) h, MRT(0-t):(6.08±0.86) h, (7.98±2.59) h and (8.31±3.35) h.Conclusion:The developed UHPLC-MS/MS method is successfully applied to pharmacokinetic study of these compounds in rats after oral administration of Oldenlandia diffusa (Willd.) extract.

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

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