学术
摘 要:
目的：建立测定人血浆中龙胆苦苷浓度的液相色谱一串联质谱法。方法：血浆加入内标咖啡因后经固相萃取处理，采用RESCEK C8柱（150mm×2．1mm，5μm）分离，流动相为甲醇-10mmol·L^-1醋酸铵溶液-乙腈（50：40：10），流速为0．2mL·min^-1。样品在三级四极杆串联质谱中经ESI源离子化后以多反应离子监测方式测定。结果：龙胆苦苷在3～5000ng·mL^-1线性良好（r=0．9985），检测限为3ng·mL^-1，回收率为94．4％～104．2％，绝对回收率为92．4％～98．O％，日内、日间变异（RSD）均≤15％，色谱峰保留时间为2．25min。结论：方法灵敏、准确、快速、特异性强，适用于中药龙胆苦苷的血药浓度测定和临床药代动力学研究。[著者文摘]
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文章出处:
《药物分析杂志》-2007年27卷2期 -157-160页
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分 类 号:
文献标识码:
A
文章编号:
0254-1793（2007）02-0157-04
Determination of gentiopicroside in human plasma by liquid chromatography- tandem mass spectrometry
FENG Yi, DENG Yuan - hui, ZENG Xing, YANG Liu, LIU Yi - ming （Department of Clinical Pharmacology,The Second Affiliated Hospital of Guangzhou University of TCM, Guangzhou,510120, China）
Abstract:
Objective：To establish an HPLC/MS/MS method in order to determine gentiopicroside in human plasma. Method：The plasma sample by solid -phase extraction with caffeine as internal standard, used the RESCEK Cs column（ 150 mm × 2. 1 mm,5 μm）as analytical column, the mobile phase consisted of methanol- 10 mmol · L^-1 ammonium acetate buffer - acetonitrile （50： 40： 10）with the flow rate of 0. 2 mL · min^-1. The sample was ionized by electrospray ionization（ESI） source in the triple quadruple tandem mass spectrometer, and was quantitated with multiple reaction monitoring mode. Results： The good linear range of gentiopicroside was 3 - 5000 ng · mL^-1 （ r = 0. 9985 ） ,the limit of quantification was 3 ng · mL^-1 ,the recovery and the absolute recovery was 94. 4% - 104.2% and 92. 4% -98.0% ,respectively. The within- day and between- day RSD were less than 15% ,the chromatography peak tR was 2. 25 min. Conclusion：The method is sensitive, accurate, rapid,, specific, suitable for determination of gentiopicroside in human plasma and clinical pharmacokinetic study.[著者文摘]
Key words:
liquid chromatography - tandem mass spectrometry; gentiopicroside; plasma concentration
基金资助:
国家863高技术研究发展计划项目（2002AA22341B）
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