离线二维液相色谱-串联质谱法检测姜黄中姜黄素类和倍半萜类化合物

Separation and characterization of curcuminoids and sesquiterpenes from C.longa L.by using 2D-LC-MS

采用二维高效液相色谱-电喷雾质谱法,以新型色谱填料ClickCD为第一维分离材料,WatersXTerraMSC18柱作为第二维,以乙腈和0.2%甲酸-水为梯度洗脱流动相,对姜黄中的姜黄素类和倍半萜类化合物进行分离鉴定.结果表明,基于不同分离机理的ClickCD和C18二维色谱系统具有分离度高、正交性好的优点,使待测化合物得到了有效分离.特别是与高灵敏度的质谱联用,可以大大提高化合物的鉴定能力.通过与对照品的色谱保留时间和质谱数据对比,并结合文献报道,共鉴定了20个姜黄素类化合物和19个倍半萜类化合物,其中27个为对照品的同分异构体.为中药化合物的表征和活性化合物的制备提供了有效方法.

A two dimensional reversed phase-reversed phase liquid chromatography tandem mass spectrometry method（2D-RP/RP-LC-MS） was successfully developed for the separation and characterization of curcuminoids and sesquiterpene from C.longa L.The 2D-RP/RP-LC-MS system consisted of a homemade Click CD column and an XTerra MS C18 column and showed good separation power and high orthogonality.Acetonitrile and 0.2% formic acid solution were employed as the elution solvent.It is demonstrated that methanol extract of C.longa L.was successfully separated based on the different separation mechanism of the two dimensions.Efficiency of compounds characterization was greatly improved for the combination of two dimensional liquid chromatography and mass spectrometry.As a result,20 curcuminoids and 19 sesquiterpenes were identified or tentatively identified based on the standard compounds and the data from previous literature.All results indicated that it would be an effective approach for the separation and characterization of Traditional Chinese Medicines and preparation of bioactive compounds.