药西瓜中三萜类成分的的LC-MS/MS分析研究

目的：运用LC-MS/MS技术研究药西瓜中葫芦素类化学成分。 方法：利用LC-MS/MS法进行分析测定。色谱条件：采用ODS-C₁₈色谱柱（250 mm×4.6 mm，5 μm），流动相为0.4%乙酸水溶液（A）-乙腈（B），梯度洗脱（0~10 min，5%B；10~20 min，5%B→15%B；20~70 min，15%B→75%B；70~75 min，75%B→5%B），流速1.0 mL·min^-1。质谱条件：ESI离子源；正负离子扫描模式；温度450℃，质量扫描范围：m/z 100~1000。 结果：以葫芦素类化合物的质谱裂解规律为指导，参照药西瓜中已报道成分的质谱数据，分析推断了药西瓜中可能含有葫芦素L-2-O-β-D-葡萄糖苷、药西瓜苷B、葫芦素E-2-O-β-D-葡萄糖苷、双氢异葫芦素B-25-乙酯和葫芦素E等8个化学成分。 结论：本实验建立的分析方法能够较全面地反映出药西瓜中葫芦素类的化学成分，为进一步开发利用该药材提供实验依据。

Objective: To investigate chemical constituents of the cucurbitacin in Fructus Colocynthis by the method of LC-MS/MS. Methods: The HPLC separation was performed on an ODS-C₁₈ column (250 mm×4.6 mm,5 μm)in gradient elute mode (0-10 min,5%B;10-20 min,5%B→15%B;20-70 min,15%B→75%B;70-75 min,75%B→5%B) with water (containing 0.4% acetic acid)(A) and acetonitrile(B) at a flow rate of 1.0 mL·min^-1.Electrospray ionization in both positive and negative ion modes was employed with ion source temperature of 450℃ and m/z range of 100-1000. Results: Guided by the mass fragmentation rule of cucurbitacin and based on the mass spectra data of the reported components in Fructus Colocynthis, eight cucurbitacin compounds were speculated in Fructus Colocynthis,including cucurbitacin L-2-O-β-D-glucopyranoside,colocynthoside B,cucurbitacin E-2-O-β-D-glucopyranoside,dihydroiso cucurbitacin B-25-acetate and cucurbitacin E etc. Conclusion: The LC-MS/MS analysis method established could comprehensively reflect the cucurbitacin compounds in Fructus Colocynthis,which provides experimental basis for further exploitation.