高效液相色谱/质联用测定大鼠血浆中双丹方活性成分

Simultaneous Determination of Active Components of Shuangdan Recipe in Rat plasma by High Performance Liquid Chromatogrpahy/Mass Spectrometry

运用LC/MS联用技术,建立同时测定大鼠血浆中丹参素、原儿茶醛、芍药苷和丹皮酚4种活性成分的分析方法。在Agilent XDB-C8柱上,以乙腈-水-0.1%醋酸为流动相,流速0.6mL/min,柱温35℃,梯度洗脱于26min内完成分析。采用选择离子监测(SIM)方式,同时以负离子模式检测丹参素、原儿茶醛、芍药苷及正离子模式检测丹皮酚。该方法简单,准确,灵敏度和专属性较好。日内精密度和日间精密度分别小于5.2%和9.9%。据此研究大鼠口服双丹方提取物后10h内血浆中上述4种物质的含量变化,结果表明:丹参素和原儿茶醛浓度在30min达到峰值,而芍药苷与丹皮酚浓度分别在60min及20min达到峰值。

A sensitive high-performance liquid chromatography/mass spectrometric （HPLC/MS） method was developed for simultaneous determination of Danshensu, protocatechuic aldehyde, paeoniflorin and paeonol in ratplasma. Agilent XDB-C8 was adopted and the column temperature was controlled at 35℃. The mobile phase was CH3CN-0. 1% CH3COOH-H2O at the flow rate of 0.6 mL/min. The separation was finished within 26 min using gradient elution. Selective ion monitoring （SIM） mode was employed. Negative electrospray ionization（ESI） was applied to analysis of Danshensu, protocatechuic aldehyde and paeoniflorin while positive way was employed for paeonol. The method is simple, accurate and specific. The intra-day and inter-day precision （RSD） was less than 5.2% and 9.9%, respectively. Danshensu, protocatechuic aldehyde, paeoniflorin and paeonol in rat plasma after intragastric administration of shuangdan recipe were determined using the proposed method. The results indicat that the tmax, of Danshensu, protocatechuic aldehyde, paeoniflofin and paeonol is 30, 30, 60 and 20min, respectively.