中国药理学通报Issue(10)：1402-1407,6.DOI:10.3969/j.issn.1001-1978.2014.10.016
LC-MS/MS法测定人血浆中羟基红花黄色素A的浓度
Determination of hydroxysafflor yellow A in human plasma by LC-MS/MS analysis
摘要
Abstract
Aim To establish a LC-MS/MS method for the determination of hydroxysafflor yellow A ( QA ) in human plasma. Methods After being added into 0. 2M ammonium acetate (1∶1,V/V), QA was extrac-ted using solid-phase extraction technique, and the eluent was directly injected into LC-MS/MS systems. Agilent ZORBAX SB C18 (3. 0 × 100 mm, 3. 5 μm) column and isocratic elution system composing of meth-anol and 0. 2 mM ammonium acetate (70 ∶ 30, V/V) provided chromatographic separation of QA and internal standard isorhamnetin-3-O-neohespeidoside ( SLS) fol-lowed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 611 . 131→490. 900 for QA and m/z 623. 032→298. 800 for SLS. Results The retention time of QA and SLS was 2. 7 min and 3. 9 min respectively, with no interference in human blank plasma. The proposed method showed good linearity over the concentration range of 8. 57 ~4185 μg·L-1 for QA with a correlation coefficient≥ 0 . 9949 . The lower limit of quantitation was 8. 570 μg ·L-1 . The intra-batch and inter-batch precision and accuracy were within 7%. The average matrix effect ranged from 115. 72% to 119. 06% with RSD less than 5%. The average extraction recovery ranged from 77. 75% to 80. 76% with RSD less than 5%. Stability of human samples after 4 h at room temperature, after the three freeze-thaw cycles and after 31 days at -70℃, and post-preparative stability of the processed sam-ples after 24 h was acceptable. Plasma samples with the concentration beyond the upper quantitation limit could be accurately determined after being diluted using 6. 25 times ( V/V ) of human blank plasma. Conclusion Our current LC-MS/MS method is sensitive, accurate and convenient, and is proved to be suitable for the sys-tematic study on clinical pharmacokinetics of QA.关键词
羟基红花黄色素A/LC-MS/MS/人血浆/血药浓度/药代动力学/SPE提取/多反应检测模式Key words
hydroxysafflor yellow A/LC-MS/MS/hu-man plasma/plasma concentration/pharmacokinetics/SPE extraction/multi-reaction monitoring mode分类
医药卫生引用本文复制引用
李长印,储继红,张军,臧雨馨,戴国梁,邹建东,居文政..LC-MS/MS法测定人血浆中羟基红花黄色素A的浓度[J].中国药理学通报,2014,(10):1402-1407,6.基金项目
国家科技部“重大新药创制”科技重大专项( No 2012ZX09303009-002) （ No 2012ZX09303009-002）
江苏省中医药领军人才( No LJ200906) （ No LJ200906）
江苏高校优势学科建设工程资助项目(2010) （2010）
