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8,2′-二异戊烯基槲皮素-3-甲醚是藏药小叶莲中的主要成分,具有较好的抗乳腺癌活性。本文首次建立了快速、灵敏的测定大鼠血浆中8,2′-二异戊烯基槲皮素-3-甲醚浓度的UPLC-MS/MS方法。以8-异戊烯基山柰酚为内标,采用waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以0.1%甲酸水–乙腈为流动相梯度洗脱,流速为0.4 mL·min–1,柱温为30oC。通过电喷雾离子化四极杆串联质谱,负离子多反应监测(MRM)模式,用于定量分析的离子反应分别为m/z451.30→177.25(8,2′-二异戊烯基槲皮素-3-甲醚)、m/z 353.25→298.15(8-异戊烯基山柰酚)。8,2′-二异戊烯基槲皮素-3-甲醚浓度为0.1–2000 ng/m L时线性关系良好(r=0.9954),高、中、低三个浓度的提取回收率在103%–115%范围内,日内、日间精密度均小于15%,准确度在–6%~15%之间。该方法简单快速灵敏,适用于检测8,2′-二异戊烯基槲皮素-3-甲醚的血药浓度并进行大鼠体内的药物动力学研究。药物动力学试验结果表明,雌性大鼠口服灌胃给药100 mg/kg的8,2′-二异戊烯基槲皮素-3-甲醚,2小时达到血浆峰浓度,生物半衰期为6.79小时,20小时内能维持一定量的血药浓度,有利于药物在生物体内产生作用。
8,2’-diisoprenyl quercetin-3-methyl ether is the main component of the Tibetan medicine lotus leaf, has good anti-breast cancer activity. This article for the first time established a fast and sensitive UPLC-MS / MS method for the determination of 8,2’-diisoprenyl qucet-3-methylether in rat plasma. Using 8-isopentenyl behenol as internal standard, a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) eluting with 0.1% formic acid in water and acetonitrile as mobile phase with a flow rate of 0.4 mL · Min-1, the column temperature is 30oC. Electron spray ionization quadrupole tandem mass spectrometry and negative ion multiple reaction monitoring (MRM) mode were used for the quantitative analysis of the ion reaction m / z 451.30 → 177.25 (8,2’-diisoprenyl quercetin -3-methyl ether), m / z 353.25 → 298.15 (8-isopentenyl kaempferol). The linearity of 8,2’-diisopentenyl quercetin-3-methylether was good at a concentration of 0.1-2000 ng / mL (r = 0.9954). The recoveries of high, medium and low concentrations of 103% -115% range, day, day precision less than 15%, accuracy of -6% to 15%. The method is simple, rapid and sensitive, and is suitable for the determination of the blood concentration of 8,2’-diisoprenyl quercetin-3-methyl ether and the pharmacokinetic study in rats. Pharmacokinetic test results showed that female rats were orally administered with 100 mg / kg of 8,2’-diisopentenyl quercetin-3-methyl ether, reached the plasma peak concentration after 2 hours, and the biological half-life was 6.79 Hour, within 20 hours to maintain a certain amount of plasma concentration, is conducive to the role of drugs in the body.