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建立高效液相色谱-串联质谱法测定大鼠血浆中淫羊藿素(ICT)。血浆样品经乙腈沉淀蛋白后,以乙腈-水-乙酸(72:28:1.5,v/v/v)为流动相,通过Dikma C18柱分离,采用电喷雾离子化四极杆串联质谱,以多反应监测(MRM)方式进行检测。用于定量分析的二级碎片离子分别为m/z387→m/z313(ICT)和m/z331→m/z315(麦黄酮,内标)。ICT血浆浓度测定方法的线性范围为2.5~1000ng·mL-1,定量限为2.5ng·mL-1。日内、日间精密度(RSD)均小于9.63%,准确度(RE)在±7.42%之内。本方法专属性强,灵敏度高,血浆用量少,适用于临床前药代动力学研究。
To establish a method for the determination of icaritin (ICT) in rat plasma by high performance liquid chromatography-tandem mass spectrometry. The plasma samples were separated by Dikma C18 column with acetonitrile-water-acetic acid (72: 28: 1.5, v / v / v) after the protein was precipitated by acetonitrile and electrospray ionization quadrupole tandem mass spectrometry Response monitoring (MRM) way to detect. Secondary fragment ions for quantitative analysis were m / z 387 → m / z 313 (ICT) and m / z 331 → m / z 315 (flavone, internal standard), respectively. The linear range of ICT plasma concentration was 2.5 ~ 1000ng · mL-1 and the limit of quantification was 2.5ng · mL-1. Day and day precision (RSD) were less than 9.63%, accuracy (RE) within ± 7.42%. The method has the advantages of high specificity, high sensitivity and less plasma dosage, and is suitable for preclinical pharmacokinetic studies.