【摘要】 目的建立人血浆中染料木素的高效液相色谱-串联质谱检测方法(HPLC/MS/MS)。方法血浆样品中加入内标物橙皮苷,用固相萃取法处理,采用AglientC18色谱柱(150mm×2.1mm,3.5μm)分离,以甲醇-10mmol·L-1乙酸铵溶液-乙腈(70∶20∶10)为流动相,流速180μL·min-1,质谱在正离子多反应监测模式(MRM)下进行特征母-子离子对信号采集,以m/z271.0→243.0(染料木素)和m/z611.2→303.2(橙皮苷)进行定量分析。结果染料木素在3～1000ng·mL-1浓度范围内线性关系良好,相关系数为r=0.9995,定量下限为3ng·mL-1,日内、日间RSD均小于10.73%(n=5),方法回收率在98.92%～104.30%。结论该方法简便、灵敏,适用于人体内染料木素血药浓度测定及临床药物动力学研究。更多还原

【Abstract】 Objective To establish a HPLC/MS/MS method for the determination of genistein in human plasma.Methods The plasma sample was deposited by solid phase extraction,with hesperidin as internal standard.The separation was performed on an Aglient C18 column(150 mm×2.1 mm,3.5 μm).The mobile phase consisted of methanol-10 mmol·L-1 ammonium acetate-acetonitrile(70 ∶20 ∶10),and the flow rate was 180 μL·min-1.Genistein was detected by MS/MS under positive electrospray ionization MRM mode.The quantification based on the peak intensity of fragment ion m/z 271.0→243.0(Genistein)and m/z 611.2→303.2(Hesperidin).Results The linear regression curve was obtained in the range of 3～1000 ng·mL-1 for genistein,the coefficient factor being 0.999 5.The lower quantification limit was 3 ng·mL-1,both intra-day RSD and inter-day RSD were less than 10.73 %(n=5).The recovery ranged 98.92 %～104.30 %.Conclusion This method is simple,sensitive,and is suitable for the measurement of plasma genistein concentrations and for clinical pharmacokinetic research.更多还原