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目的:建立大鼠血浆中卡瓦内酯麻醉椒苦素的液相色谱质谱联用定量分析方法,并用于大鼠体内药物动力学研究。方法:采用Waters Symmetry Shield C8(3.0 mm×150 mm,5.0μm)色谱柱,流动相为乙腈-0.2%甲酸溶液(60∶40,v/v)。三重四极杆质谱仪进行多反应监测(MRM)模式,电喷雾离子源(ESI)正离子检测。生物样品预处理采用乙酸乙酯液-液萃取,考察麻醉椒苦素灌胃给药后,大鼠体内药物动力学特征。结果:在大鼠血浆中麻醉椒苦素浓度与峰面积比呈良好线性关系(r=0.9998),线性范围为10～20000μg·L-1,定量下限为10μg·L-1,样品分析时间为5.5 min。日内、日间精密度(RSD)均小于5.3%,准确度在±10.3%之内。SD大鼠灌胃给药麻醉椒苦素120 mg·kg-1后,平均血药峰浓度为8.92 mg·L-1,血药浓度达峰时间平均为4.00 h。结论:所建立的HPLC-MS/MS定量分析方法特异、快速、灵敏,可用于麻醉椒苦素临床前药物动力学研究。
OBJECTIVE: To establish a quantitative method for the quantitative analysis of anesthesia peppervetone in rat plasma by LC-MS and to study the pharmacokinetics of rat plasma in rats. Methods: A Waters Symmetry Shield C8 (3.0 mm × 150 mm, 5.0 μm) column was used with a mobile phase of acetonitrile-0.2% formic acid (60:40, v / v). Triple quadrupole mass spectrometry for multiple reaction monitoring (MRM) mode, electrospray ionization (ESI) positive ion detection. Biological samples were pre-treated with ethyl acetate liquid-liquid extraction to study the pharmacokinetic characteristics of rats after intragastric administration of peppermint. Results: There was a good linear relationship between the concentration of peppermint and peak area in rat plasma (r = 0.9998), the linear range was 10 ~ 20000μg · L-1, and the lower limit of quantification was 10μg · L-1. The analysis time was 5.5 min. Intra-day and inter-day precision (RSD) were less than 5.3%, accuracy within ± 10.3%. After intragastric administration of 120 mg · kg-1 of pepelitazone, the average peak plasma concentration of 8.92 mg · L-1 and the mean peak plasma concentration of 4.42 h in SD rats. Conclusion: The established HPLC-MS / MS method is specific, rapid and sensitive and can be used to study the preclinical pharmacokinetics of peppermint.