摘要
目的：建立LC-MS/MS法同时测定大鼠血浆中环磷酸腺苷（cAMP）、环磷酸鸟苷（cGMP）的浓度。方法：采用RRHD Eclipse Plus C18色谱柱（3.0 mm×100 mm,1.8μm）,柱温为25℃,以水（含0.1%甲酸）-乙腈（90∶10）为流动相,流速为0.3m L·min-1。2种被测成分的监测反应质荷比分别为330.10→136.00（cAMP）、346.05→152.00（cGMP）,内标化合物的监测反应质荷比为277.28→152.00（恩替卡韦）。结果：cAMP、cGMP的线性范围分别为0.010 1-1 010.00 ng·m L-1、0.010 0-1 000.00 ng·m L-1（r≥0.999 0）,最低检测浓度分别为0.010 1、0.010 0 ng·m L-1。日内、日间RSD均小于15%,重复性好。采用LC-MS/MS方法测定大鼠血浆中cAMP、cGMP的浓度分别为（1.92±0.26）ng·m L-1和（3.61±0.40）ng·m L-1。结论：该方法灵敏、快捷、准确,专一性强,可用于药物代谢的分析研究及中医药作用机制研究。
Objective：To establish a ultra-high liquid chromatography-tandem quadrupole mass spectrometry（LCMS/MS） method for simultaneous determination of adenosine 3 ＇,5＇-cyclic monophosphate（cAMP） and guanosine3＇,5＇-cyclic monophosphate（cGMP） in rat plasma.Methods：Entecavir was used as the internal standard for the determination of the two active substances in rat plasma.The chromatographic analysis was carried out by RRHD Eclipse Plus C18column（3.0 mm × 100 mm,1.8 μm） and the column temperature was 25 ℃.The mobile phase consisted of water（containing 0.1% formic acid）-acetonitrile（90 ∶ 10） at a flow rate 0.3 m L·min-1.Detection and quantification were performed by mass spectrometry in multiple reaction monitoring mode with m/z 330.10 →136.00 for cAMP,m/z 346.05 → 152.00 for cGMP and m/z 277.28 → 152.00 for entecavir,respectively.Results：The linear ranges were 0.010 1-1 010.00 ng·m L-1for cAMP and 0.010 0-1 000.00 ng·m L-1for cGMP（r≥0.999 0）.The minimum detectable concentrations were 0.010 1 ng m L-1and 0.010 0 ng·m L-1,respectively.The RSD was less than 15%,and the repeatability was good.The concentrations of cAMP and cGMP in rat plasma were（1.92 ± 0.26） ng·m L-1and（3.61 ± 0.40） ng·m L-1,respectively.Conclusion：This method is successfully applied for the determination.It is rapid,simple,sensitive and specific,which can be used as an effective method for the drug metabolism studies and researches on the mechanism of action of traditional Chinese medicine.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第6期1022-1026,共5页
Chinese Journal of Pharmaceutical Analysis
基金
江苏高校优势学科建设工程资助项目
南京中医药大学中药学一级学科开放课题资助(2011ZYX6-006)
