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建立同时测定大鼠灌胃及静注给予浙贝母提取物后血浆中贝母素甲及贝母素乙含量的HPLC-MS/MS分析方法,并计算2种生物碱在大鼠体内的药代动力学参数。血浆样品经乙酸乙酯液-液萃取后,以乙腈-10mmol·L-1甲酸铵水溶液(35∶65)为流动相,Luna C18色谱柱(150mm×2mmID,3μm)分离,采用电喷雾离子化源(ESI)三重四极杆串联质谱,以多反应监测模式(MRM)进行检测,检测离子对分别为m/z432.4→414.4(贝母素甲)、m/z430.4→412.4(贝母素乙)和m/z237.1→194.2(内标,卡马西平)。贝母素甲及贝母素乙均在0.8~800ng·mL-1内呈良好线性关系,提取回收率分别为94.1%~105.3%和85.8%~98.6%。方法的精密度、准确度和稳定性均符合要求。结果显示,该法选择性强、灵敏度高、操作简便,适用于贝母素甲、贝母素乙的大鼠药代动力学研究。
To establish a HPLC-MS / MS method for the simultaneous determination of plasma midgutin and peiminine B after gavage and intravenous injection of Fritillaria thunbergii in rats, and to calculate the contents of two alkaloids in rats Generational dynamics parameters. The plasma samples were separated by liquid-liquid extraction with ethyl acetate and separated on a Luna C18 column (150mm × 2mmID, 3μm) using acetonitrile-10mmol·L-1 ammonium formate aqueous solution (35:65) as mobile phase. Electrospray ionization (ESI) triple quadrupole tandem mass spectrometry (MS-MS / MS) was used to detect the ion pairs in m / z 432.4 → 414.4 (m), m / z 430.4 → 412.4 Maternal B) and m / z 237.1 -> 194.2 (internal standard, carbamazepine). There was a good linear relationship between peptone and peiminine in the range of 0.8 ~ 800 ng · mL-1. The recoveries were 94.1% -105.3% and 85.8% -98.6%, respectively. The precision, accuracy and stability of the method are in line with the requirements. The results show that this method is selective, sensitive and easy to operate. It is suitable for the pharmacokinetic study of rats in Fritillaria and Fritillaria.