论文部分内容阅读
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 in organism with very low concentration to play a good effect, accurate determination of its plasma concentration of its pharmacological properties of great significance. A method for the rapid determination of berberine in plasma by high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed. The method was based on a Waters XTerraTM MSC18 column (2.1 × 50mm, 3.5μm) with a column temperature of 25 ℃ and 0.2% acetic acid in water Phase gradient elution, flow rate of 0.2mL / min, phenytoin as an internal standard. The mass spectrometry was electrospray ionization source, quantitative analysis was performed with selective reaction monitoring mode, and plasma samples were directly precipitated with acetonitrile. The results showed that berberine had a good linearity in the range of 0.01-0.5 μg / mL with the lowest detection concentration of 5 ng / mL (S / N = 3). Day and day RSDs were less than 15% (n = 5). The method established in this paper is simple, high sensitivity, short analysis time, suitable for the monitoring of berberine concentration and pharmacokinetics.