UPLC—MS／MS法同时测定消栓通络方中18种成分的含量

消栓通络方是临床应用广泛的中药复方制剂。本文建立了一种可同时检测该方剂中18种活性成分的超高效液相．串联四级杆质谱方法。采用多反应监测（MRM）模式测定，离子化方式选择ESI＋和NESI-。利用BEHC18（2．1mm×100mm，1．7μm）色谱柱进行分离，甲醇-0．1％甲酸溶液0．2mL／min梯度洗脱。18种活性成分测定的线性范围多在0．001-0．5μg／mL之间，r值在0．9896-9996之间：高、中、低3个水平日内、日问精密度RSD均〈15％；室温24h稳定性RSD〈15％。应用该方法对4种不同剂型的市售消栓通络方制剂18种活性成分进行了测定，结果显示该方法快速、准确、灵敏、重现性好，可用于消栓通络方制剂的质量控制。

Simultaneous quantification of eighteen constituents in traditional Chinese medicine XiaoShuanTongLuo by UPLC-MS/MS

XiaoShuanTongLuo （XSTL） is an important multi-herbal formula widely used as a traditional Chinese medicine （TCM）. In this paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometric method （UPLC-ESI-MS/MS） was developed for the simultaneous identification and quantification of 18 chemical constituents in the extract of XSTL. The analysis was performed in multiple-reaction monitoring （MRM） mode using positive and negative electrospray ionization （ESI）. A BEH C18 （2.1 mm× 100 mm, 1.7 μm） column with a gradient mobile phase of methanol-0.1% aqueous formic acid solution at a flow rate of 0.2 mL/min was used for separation. The standard curves of most components showed good linearity over the concentration range of 0.001-0.5 μg/mL with r = 0.9896-0.9996. The relative standard deviations （RSD） of intra-day and inter-day precision were all lower than 15% at low, middle, and high concentration levels. The RSD of stability analysis in 24 h were also lower than 15%. The validated method was employed to quantify 18 active components simultaneously in four different commercial brands of XSTL products in various dosage forms. The developed method was rapid, accurate, sensitive, and reproducible for the quality control of XSTL.