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目的建立高效液相色谱/四极杆-静电场轨道阱高分辨质谱(HPLC-Q-HR/MS)方法,研究大黄素在正常与脑缺血大鼠体内的药动学规律。方法采用HPLC-Q-HR/MS内标法测定大黄素血药浓度,色谱柱为XBridge~(TM) C_(18)柱(150 mm×2.1mm,5μm),柱温30℃;流动相为3 mmol/L乙酸铵-甲醇,梯度洗脱,梯度洗脱程序为0～2 min,30%甲醇;2～10 min,30%～60%甲醇;10～13 min,60%～30%甲醇;体积流量为0.3 m L/min;进样体积为5μL;质谱条件:离子源为加热电喷雾离子化源(HESI),扫描方式为全扫模式,负离子模式检测。以DAS 3.0软件拟合计算药动学参数。结果大黄素在正常与脑缺血大鼠血浆中的主要药动学参数分别为AUC_(0-∞)(605.63±163.66)、(1 107.78±191.11)ng?h/m L,C_(max)(81.96±20.72)、(91.65±16.82)ng/m L,V_Z/F(851.03±97.30)、(1 051.87±119.88)L/kg,t_(1/2)(10.31±1.61)、(23.13±3.56)h,t_(max)(0.75±0.22)、(0.75±0.16)h。结论该法操作简便、分析速度快速、灵敏,适用于大黄素在大鼠体内的药动学研究。
OBJECTIVE To establish a HPLC-Q-HR / MS method for the determination of pharmacokinetics of emodin in normal and ischemic rats. Methods The emodin concentration was determined by HPLC-Q-HR / MS. The column was XBridge C18 column (150 mm × 2.1 mm, 5 μm) with a column temperature of 30 ℃. The mobile phase was 3 mmol / L ammonium acetate-methanol gradient elution, the gradient elution program is 0 ~ 2 min, 30% methanol; 2 ~ 10 min, 30% ~ 60% methanol; 10 ~ 13 min, 60% ~ 30% methanol ; Volume flow of 0.3 m L / min; injection volume of 5 μL; mass spectrometry conditions: ion source for heating electrospray ionization source (HESI), scanning mode for the full scan mode, negative ion mode detection. Pharmacokinetic parameters were calculated using DAS 3.0 software. Results The main pharmacokinetic parameters of emodin in normal and ischemic rats were AUC 0-∞ (605.63 ± 163.66), (1 107.78 ± 191.11) ng · h / m L, C max, (81.96 ± 20.72), (91.65 ± 16.82) ng / m L, V_Z / F (851.03 ± 97.30), (1051.87 ± 119.88) L / kg and t 1/2 (10.31 ± 1.61) 3.56) h, t max (0.75 ± 0.22), (0.75 ± 0.16) h. Conclusion The method is simple, rapid, sensitive, suitable for pharmacokinetic studies of emodin in rats.