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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 a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of naringin in plasma and study the pharmacokinetics of naringenin and glucuronic acid conjugates in rats. Methods The chromatographic column was a Shimpack ODS C18 column (2.3 mm × 75 mm, 3 μm). The mobile phase consisted of a gradient of 0.1% acetic acid in water and methanol. The flow rate was 0.2 mL · min-1. M / z 271.1 → 151.0 (naringenin), 301.2 → 164.1 (hesperetin, internal standard). Results The linearity of naringin plasma spiked in 10 ng · mL-1 ~ 4 μg · mL-1 was good (r = 0.999 7). The recoveries of high, medium and low concentrations of naringenin were between 85% and 115%. The method was used to systematically study the plasma concentrations of naringenin and glucuronic acid conjugates in rats administered with different dosages. Conclusion The method is fast, sensitive and reproducible. Naringenin peak in the blood faster, and most of the blood glucuronic acid, a small part of the existence of free form.