高效液相色谱-质谱联用法测定大鼠血浆中五味子醇乙的浓度及其应用

Determination of Gomisin A in Rat Plasma by HPLC-MS and Its Application

目的建立快速、灵敏的高效液相色谱-质谱法测定大鼠血浆中五味子醇乙的浓度,并研究其在大鼠体内的药动学变化规律。方法以地西泮为内标,血浆样品经乙醚萃取后进行高效液相色谱-质谱分析,采用Hypersil-C18色谱柱(150 mm×4.6 mm,5μm),甲醇-水(72∶28)为流动相,检测离子为399.00(五味子醇乙[M+H-H2O]+),284.90(内标地西泮[M+H]+)。结果血浆标准曲线线性范围为5.0～250 ng/mL(r=0.995 7),最低定量下限为5.0 ng/mL。五味子醇乙的提取回收率不小于78.80%,高、中、低3种浓度的日内、日间精密度RSD均小于15%(n=6)。结论该方法选择性强、灵敏度高,适用于大鼠血浆中五味子醇乙浓度测定和临床药动学研究。

Objective To develop a fast and sensitive HPLC-MS method for the determination of the concentration of gomisin A in rat plasma and study the pharmacokinetics in rats.Methods Plasma was extracted by diethyl ether,and then separated on Hypersil-C18（150 mm×4.6 mm,5 μm）with a mobile phase of method-water（72 ∶28）.Diazepam was used as the internal standard.m/z 399.00 and m/z 284.90 were used to qualify gomisin A and diazepam,respectively.Results The linear calibration curve was obtained from 5.0 to 250 ng/mL（r=0.995 7）.The limit of quantification was 5.0 ng/mL.The recovery for gomisin A was greater than or equal to 78.80%,the inter-day and intra-day precision（RSD） were all less than 15%（n=6）.Conclusion The method is selective,sensitive,and suitable for the preclinical pharmacokinetics of gomisin A.