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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,5μm),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 study the chemical constituents of cucurbitacin in watermelon by LC-MS / MS. Methods: Analytical determination by LC-MS / MS method. The chromatographic conditions were as follows: ODS-C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of 0.4% acetic acid in water and gradient elution (0-10 min, 5% 20 min, 5% B → 15% B; 20-70 min, 15% B → 75% B; 70-75 min, 75% B → 5% B) at a flow rate of 1.0 mL · min -1. Mass spectrometry conditions: ESI ion source; positive and negative ion scanning mode; temperature 450 ℃, mass scan range: m / z 100 ~ 1000. Results: Based on the mass spectrometric cleavage of cucurbitacin compounds, with reference to the mass spectrometry data of reported constituents in watermelon, it was concluded that cucurbitacin L-2-O-β-D-glucoside, Glycoside B, cucurbitacin E-2-O-β-D-glucoside, dihydro-isobuciferin B-25-ethyl ester and cucurbitacin E and other eight chemical constituents. Conclusion: The analytical method established in this experiment can reflect the chemical constituents of cucurbitacins in watermelon more fully, and provide the experimental basis for further development and utilization of the medicinal materials.