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目的:建立高效液相色谱-质谱法(UPLC-MS)测定大鼠口服线叶菊有效部位后血浆中异荭草素、异鼠李素-3-O-β-D-葡萄糖苷和东莨菪苷的含量,研究这3个指标性成分在大鼠体内的药代动力学行为。方法:采用ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.7μm),流动相0.1%甲酸水溶液(A)-0.1%甲酸乙腈溶液(B)梯度洗脱(0~2 min,98%A;2~6 min,98%~30%A;6.0~7.6 min,30%~40%A;7.6~8.0 min,40%~2%A;8~10 min,2%A;10~12 min,2%~98%A),流速0.4 m L·min-1,柱温40℃;电喷雾离子源(ESI),多反应监测(MRM)模式。采用单次给药法,大鼠按1.0 g·kg-1灌胃给予线叶菊有效部位,通过负离子模式测定血浆中异荭草素、异鼠李素-3-O-β-D-葡萄糖苷和东莨菪苷的含量。结果:各成分的线性关系良好(R2>0.997),各成分的提取回收率在80.87%~93.75%;日内、日间精密度RSD均<15%。3种成分的达峰时间(tmax)分别为(32.40±4.16),(30.00±4.80),(20.10±5.10)min,药峰浓度(Cmax)分别为(31.80±5.46),(28.00±2.54),(20.33±1.17)μg·L~(-1),药时曲线下面积(AUC0-t)分别为(37.80±3.94),(48.83±3.05),(32.40±2.64)μg·min·L~(-1),消除半衰期(t1/2β)分别为(114.06±22.19),(126.12±19.38),(148.14±24.10)min。结论:建立的UPLC-MS精密、准确,能够同时测定生物样品中异荭草素等3种成分的血药浓度。这3种成分进入体内及吸收的速度较快,但吸收情况并不理想。
OBJECTIVE: To establish a method for the determination of isohumulone, isorhamnetin-3-O-β-D-glucoside and scopolamine in rats by high performance liquid chromatography-mass spectrometry (UPLC-MS) The pharmacokinetic behavior of these three index components in rats was studied. Methods: The mobile phase consisted of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile (B) with gradient elution (0-2 min, 98% A ; 2-6 min, 98% -30% A; 6.0-7.6 min, 30-40% A; 7.6-8.0 min, 40-2% A; 8-10 min, 2% A; , 2% ~ 98% A), flow rate 0.4 m L · min-1, column temperature 40 ℃; electrospray ionization source (ESI) and multiple reaction monitoring (MRM) In the single administration method, rats were given gavage at the dose of 1.0 g · kg-1, and the content of isoorientin, isorhamnetin-3-O-β-D-glucoside And scopolamine content. Results: The linearity of each component was good (R2> 0.997). The recovery rates of the components were in the range of 80.87% -93.75%. The intra-day and inter-day RSDs were all <15%. The peak time (tmax) of the three components were (32.40 ± 4.16), (30.00 ± 4.80) and (20.10 ± 5.10) min, and the peak drug concentrations were 31.80 ± 5.46 and 28.00 ± 2.54, , (20.33 ± 1.17) μg · L -1, respectively. The area under the curve (AUC0-t) was (37.80 ± 3.94), (48.83 ± 3.05) and (32.40 ± 2.64) μg · min ~ (-1), and the elimination half-life (t1 / 2β) were (114.06 ± 22.19), (126.12 ± 19.38) and (148.14 ± 24.10) min, respectively. Conclusion: The established UPLC-MS is accurate and accurate and can simultaneously determine the plasma concentrations of three components such as isohumulone in biological samples. The three components into the body and absorbed faster, but the absorption is not ideal.