高效液相色谱-串联质谱法分析姜黄中微量的姜黄素类化合物

建立了同时检测中药姜黄中3种微量的姜黄素类化合物的高效液相色谱-电喷雾串联质谱分析方法。姜黄根茎经乙醇超声提取后,无需其他处理可直接进样分析。以Microsorb C18色谱柱(250 mm×4.6 mm,5 μm)分离,乙腈和0.1%甲酸水梯度洗脱,在多反应监测模式(MRM)下对目标成分进行定性分析。利用质谱碎裂规律,分别对每个目标成分同时监测8个母离子/特征子离子对的反应过程,首次从姜黄中发现了3个微量的姜黄素类化合物成分。一次性完成了目标成分的同时定性,方法的检出限为0.2 μg/L。结果表明,该方法具有简便、快速、准确、灵敏度高的优点,适用于中药复杂体系中姜黄素类化合物的分析检测。

Analysis of minor curcuminoids in Curcuma longa L. by high performance liquid chromatography-tandem mass spectrometry

A high performance liquid chromatography-tandem mass spectrometric method has been developed for the simultaneous analysis of three minor curcuminoids in the crude extract of Curcuma longa L. After ultrasonic extraction with ethanol, the sample was separated on a Microsorb C18 column (250 mm×4.6 mm, 5 μm) with the gradient elution of acetonitrile and 0.1% (v/v) formic acid aqueous solution as mobile phase, then detected by electrospray ionization tandem mass spectrometry in multi-reaction monitoring (MRM) mode. On the basis of analysis of the fragmentation patterns, the identification of the minor ones was achieved in a single experiment using MRM with 8 precursor-product ion transitions for each component. Using this technique, the three minor curcuminoids were observed in C. longa L. for first time and the limit of detection was 0.2 μg/L. The experimental results show that this method is simple, rapid, accurate, sensitive and suitable for the analysis of curcuminoids in the complex samples of traditional Chinese medicine.