期刊文献+

HPLC-MS/MS测定人体内齐墩果酸血药浓度 被引量:1

HPLC-MS/MS Determination of Oleanolic Acid in Human Plasma
原文传递
导出
摘要 目的建立快速、灵敏的高效液相色谱-串联质谱(HPLC-MS/MS)法测定人血浆中的齐墩果酸。方法血浆样品定量加入内标液,经乙酸乙酯液液萃取后,以甲醇-0.1%醋酸铵缓冲溶液(93:7)为流动相,采用Zorbax Extend-C18(4.6mm×250mm,5μm)柱分离。使用电喷雾离子化,负离子SRM检测。用于定量的离子反应分别为m/z455.1→455.3(齐墩果酸);m/z469.1→469.3(内标甘草次酸)。结果测定血浆中齐墩果酸的线性范围为0.1~40.0μg.L-1,定量限为0.1μg.L-1,批内、批间精密度(RSD)均小于20.0%,方法学回收率94.0%~102.0%,符合相关规定。单个样品的分析时间为6.5min。本法已用于齐墩果酸口服制剂的人体生物等效性研究。结论本方法灵敏度高,选择性强,分析测试时间较短,适用于人血浆样品中齐墩果酸的测定。 OBJECTIVE To develop and validate a method for the determination of oleanolic acid in human plasma by HPLC-MS/MS.METHODS The plasma sample was extracted with ethyl acetate,then separated on a Zorbax Extend-C18(4.6 mm×250 mm,5 μm)column using methanol-0.1%ammonium acetate (93:7) as the mobile phase.The triple quadrupole mass spectrometry was applied.Quantitation was performed using positive ion selected reaction monitoring (SRM) of the transitions of m/z 455.1→455.3 and m/z 469.1→469.3 for oleanolic acid and the internal standard glycyrrhetinic acid,respectively.RESULTS The linear calibration curves were obtained in the concentration range of 0.1-40.0 μg·L^-1.The limit of quantification was 0.1 μg·L^-1.The intra-day and inter-day relative standard deviation over the entire concentration range was below 20.0%.The accuracy was 94.0%-102.0%.Each sample was finished within 6.5 min.The method was applied to evaluate the bioequivalence of two oleanolic acid tablet formulations in healthy volunteers.CONCLUSION This method is sensitive,selective,rapid and suitable for the determination of oleanolic acid in human plasma.
出处 《中国药学杂志》 CAS CSCD 北大核心 2010年第10期772-775,共4页 Chinese Pharmaceutical Journal
关键词 齐墩果酸 高效液相色谱-串联质谱法 血浆药物浓度 oleanolic acid HPLC-MS/MS plasma drug concentration
  • 相关文献

参考文献7

二级参考文献49

  • 1吴皓,蔡宝昌,郑培新,赵春忠,袁铸人.炮制对马钱子中生物碱的影响[J].中国中药杂志,1994,19(5):277-279. 被引量:21
  • 2牟晨晔.几种炮制方法对马钱子士的宁含量的影响[J].现代应用药学,1995,12(2):26-27. 被引量:4
  • 3唐芳,杨绍华,刘家稳,冯裕,李焕德.齐墩果酸滴丸的制备及其体外溶出度研究[J].中南药学,2005,3(6):352-354. 被引量:10
  • 4.中国药典(一部)[M].,2000.37.
  • 5代龙 叶定江.从士的宁的含量看马钱子的炮制[J].山东中医杂志,1990,9(3):39-39.
  • 6Lowe SW, Lin AW. Apoptosis in cancer [J]. Carcinogenesis , 2000,21(3):485-495.
  • 7Myoung SK,Ho JK,You ML ,et al. Histone deacetylases induce angiogenesis by negative regulation of tumor suppressor genes [J]. Nat Med,2001, 7:437~443.
  • 8Kirlin WG, Cai J, Delong MJ, et al. Dietary compounds that induce cancer priventive phase 2 enzymes activate apoptosis at comparable doses in HT-29 colon carcinoma cells [J]. J Nutr, 1999, 129 : 1827~1835.
  • 9Ruemmele FM, Schwartz S , Seidman EG, et al. Butyrate induced Caco-2 cell apoptosis is mediated via the mitochondrial pathway [J]. Gut , 2003 , 52 (1) :94~100.
  • 10Colquhoun A, Ramos KL, Schumacher RI. Eicosapentaenoic acid and docosahexaenoic acid effects on tumour mitochondrial metabolism, acyl CoA metabolism and cell proliferation [J]. Cell Biochem Funct, 2001 ,19(2) :97~105.

共引文献224

同被引文献29

引证文献1

二级引证文献11

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部