摘要
目的建立柚皮素血浆浓度的高效液相色谱-串联质谱（HPLC-MS/MS）分析方法,研究柚皮素及其葡萄糖醛酸结合物在大鼠体内的药动学。方法色谱柱为Shimpack ODS C18柱（2.3 mm×75 mm,3μm）,流动相为体积比0.1%醋酸水溶液和甲醇,梯度洗脱,流速0.2 mL·min-1,MRM负离子模式扫描,定量离子对为m/z 271.1→151.0（柚皮素）,301.2→164.1（橙皮素,内标）。结果柚皮素血浆加标样品在10 ng·mL-1~4μg·mL-1内线性关系良好（r=0.999 7）,高、中、低浓度回收率均在85%~115%之间。采用该方法系统研究了灌胃给药时不同给药剂量下大鼠的柚皮素及其葡萄糖醛酸结合物的血药浓度情况。结论所建方法快速,灵敏,重现性好。柚皮素在血中达峰较快,且大部分与血液中的葡萄糖醛酸结合,少部分以游离形式存在。
OBJECTIVE To establish an LC-MS /MS method for determination of naringenin and its glucuronic acid conjugate in rat plasma. METHODS A Shimpack ODS C18column（ 2. 3 mm × 75 mm,3 μm） was used with a mobile phase consisting of 0. 1% acetic acid solution and methanol at the flow rate of 0. 2 mL·min- 1. The detection mode was MRM,and the precursor / product ion pair was m / z 271. 1→151. 0 for naringenin and m / z 301. 2→164. 1 for the IS. RESULTS The calibration curve was linear in the range of 0. 01- 4 μg·mL- 1（ r =0. 999 7） for naringenin. The average recoveries at high,medium,and low concentrations were between 85%- 115%. The method was used to determine the plasma concentration of naringenin after gastric gavages of different dosages to Wister rats. CONCLUSION The method is rapid,sensitive and reproducible. Naringenin,reaching peak concentration quickly, has low concentration in plasma and most became its glucuronic acid conjugate.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2014年第10期864-868,共5页
Chinese Pharmaceutical Journal
基金
"重大新药创制"国家科技重大专项(2012ZX09301002-001-006)
