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目的:建立HPLC-MS分析方法同时测定大鼠血浆中的乌头碱、新乌头碱、次乌头碱含量,并用于研究大鼠口服附子煎液后乌头碱、新乌头碱、次乌头碱的药动学。方法:血浆经氨水碱化后用醋酸乙酯进行液-液萃取。色谱柱为Alltima C18柱(250mm×4.6mm,5μm),流动相为甲醇-10mmol.L-1醋酸铵水溶液(75∶25)。质谱检测方式为选择性离子监测,选择监测的离子为m/z646.45(乌头碱),m/z632.38(新乌头碱),m/z615.64(次乌头碱)和m/z336.60(盐酸小檗碱,内标)。结果:血浆中乌头碱在0.05~5μg.L-1、新乌头碱在0.5~50μg.L-1、次乌头碱在2.5~250μg.L-1范围内线性关系良好,定量限为0.05μg.L-1,血浆中的平均提取回收率高于90%,批内和批间精密度均小于15%。结论:本法灵敏、可靠、简便,适用于乌头碱、新乌头碱、次乌头碱的药动学研究。
OBJECTIVE: To establish an HPLC-MS method for the simultaneous determination of aconitine, mesaconitine and hypaconitine in rat plasma and to study the effects of aconitine, mesaconitine, Aconitine pharmacokinetics. Methods: The plasma was alkalized by ammonia water and extracted with ethyl acetate. The column was Alltima C18 column (250 mm × 4.6 mm, 5 μm) and the mobile phase was methanol-10 mmol·L-1 ammonium acetate aqueous solution (75:25). The mass spectrometry detection method was selective ion monitoring. The ions monitored for selection were m / z 646.45 (aconitine), m / z 632.38 (mesaconitine), m / z 615.64 (hypaconitine) and m /z336.60 (berberine hydrochloride, internal standard). Results: There was a good linear relationship between the concentration of aconitine in the plasma of 0.05 ~ 5μg.L-1, the mesaconitine of 0.5 ~ 50μg.L-1 and hypaconitine in the range of 2.5 ~ 250μg.L-1. The limits of quantitation 0.05μg.L-1, the average recovery rate of plasma was higher than 90%, intra-batch and inter-batch precision were less than 15%. Conclusion: This method is sensitive, reliable and simple, suitable for aconitine, mesaconitine, hypaconitine pharmacokinetics.