LC-MS/MS法测定人血浆中ASE浓度

Determination of armillarisin succinate ester in human plasma by LC-MS/MS

目的 建立LC-MS/MS法测定人血浆中亮菌甲素琥珀酸单酯（ASE）的方法.方法 ZorbaxSB-C18色谱柱（30 mm ×2.1 mm,3.5 μm）,流动相：甲醇-20 mM乙酸铵水溶液梯度洗脱,柱温：30℃,流速：0.4 mL/min.以补骨脂甲素为内标,在负离子模式下,采用选择离子监测（SIM）方式,监测离子对分别为m/z333→233和m/z 323→221.结果 ASE LC-MS/MS法的最低检测浓度为0.5 ng/mL,在0.01 ～ 10.0μg/mL（r =0.9914）内线性关系良好.该方法下ASE日内精密度RSD分别为2.18％ ～5.62％,日间精密度RSD分别为4.72％ ～6.23％.方法回收率分别为93.2％～109.2％.结论 本试验建立的方法准确、快速、简便,适用于ASE体内血药浓度和生物等效性的测定.

Objective To determinate the armillarisin succinate ester （ASE）in plasma by LC-MS/MS.Methods The separation was carried out on a Zorbax SB-C18 （30 mm × 2.1 mm,3.5 μm） column and methanol -20 mM ammonium acetate aqueous as mobile phase using gradient elute at flow rate of 0.4 mL/min.Bavachin was employed as the internal standard.In negative scanning mode,quantification was performed using the transitions m/z 333→233 and m/z 323→221,respectively.Results The limits of detection was 0.5 ng/mL.The concentration of ASE showed a linear plot in the range of 0.01 ～ 10.0 μg/mL（r =0.991 4）.The inter-day and intra-day relative standard deviation（RSD） for the method were 2.18％ ～ 5.62％ and 4.72％ ～ 6.23％,respectively.The extraction recovery rate was 93.2％ ～ 109.2％.Conclusion The method is proved to be accurate,sensitive and reliable.It is suitable for the determination in human plasma of ASE.