摘要:
清肝散结汤(QGSJ)是由14味不同中药组成的复方制剂,基于长期的实验观察和临床经验以不同组合成方用于肝癌的治疗.本研究建立了一种基于加速溶剂萃取(ASE)结合高效液相色谱-电喷雾飞行时间质谱(HPLC-ESI-TOF MS)的方法同时测定清肝散结汤中29种化学成分.使用70%乙醇作为提取溶剂,提取温度100 ℃,静态萃取时间5 min,提取2次,以上条件采用正交设计和主成分分析进行优化.HPLC分离采用Kromasil C18色谱柱,梯度洗脱.TOF MS在负离子模式下检测,质量扫描范围m/z 100～1 100.结果表明:清肝散结汤中29种成分具有良好的线性关系(r>0.994)和日内、日间精密度(RSD<5%);提取回收率在96.5%～104.5%之间.该方法快速、可靠,适用于复方中药的定量评价.
Abstract:
QingGanSanJie decoction (QGSJ), which consists of 14 different herbs, is a multiherbal formula for liver cancer that is administered in different combinations based on experimental observations and clinical experiences from long-term applications.A method based on accelerated solvent extraction (ASE) followed by high-performance liquid chromatography (HPLC) coupled with electrospray time-of-flight mass spectrometry (ESI-TOF MS) were established for simultaneous determination of 29 chemical components in QGSJ.The operational parameters of ASE, including the extraction solvent (70% ethanol), extraction temperature (100 ℃), static extraction time (5 min), and extraction cycles (two cycles) were optimized by orthogonal design and principal component analysis.HPLC separation was performed on a Kromasil C18 HPLC column with a linear gradient mobile phase system.TOF MS was set in negative ion mode with a detector range of m/z 100-1 100.The results show that 29 compounds in the QGSJ have good linearity (r>0.994), and intra-day and inter-day precision (relative standard deviation) are less than 5%.The extraction recoveries of the 29 compounds range from 96.5% to 104.5%.The method is rapid and reliable, which is suitable for the quantitative evaluation of multiherbal traditional Chinese medicine.
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