摘要
小檗碱在生物体内以极低的浓度发挥着良好的疗效,准确测定其血药浓度对其药理学性质的研究具有重要意义。本文建立了高效液相色谱-质谱联用快速测定血浆中小檗碱浓度的方法,采用Waters XTerraTM MSC18色谱柱(2.1×50mm,3.5μm),柱温25℃,以0.2%醋酸水溶液-乙腈为流动相梯度洗脱,流速为0.2mL/min,以苯妥英为内标。质谱采用电喷雾电离源,以选择反应监测模式进行定量分析,血浆样品用乙腈直接沉淀处理。结果表明,小檗碱在0.01~0.5μg/mL浓度范围线性关系良好,最低检测浓度为5ng/mL(S/N=3)。日内、日间RSD均小于15%(n=5)。本文建立的方法操作简单、灵敏度高、分析时间短,适用于小檗碱血药浓度监测及药代动力学研究。
Berberine(BBR) exhibits great pharmacological effects with very low concentration in vivo.A high performance liquid chromatography electrospray mass spectrometry method for rapid determination of BBR in plasma has been established.The analysis was carried on a Waters XTerraTM MS C18 column(2.1×50mm,3.5μm).The column temperature was 25℃,with linear gradient elution using 0.2% acetic acid solution and acetonitrile,and the flow rate was 0.2mL /min.The quantitation was done by selected reaction recording(SRM) mode of electrospray ionization(ESI),with phenytoin as internal standard.Plasma was deposited by acetonitrile directly.The linear range was 0.01 ~ 0.5μg /mL for BBR,and the detection limit was 5ng /mL(S/N=3);both intra-and inter-day RSD were less than 15%(n=5).The method is accurate,sensitive,simple,and suitable for study of therapeutic drug monitoring and pharmacokinetic.
出处
《化学通报》
CAS
CSCD
北大核心
2010年第8期757-760,共4页
Chemistry