UPLC-ESI-Q-TOF-MS Analysis of Xanthones in Swertia Chirayita
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摘要: 目的 建立印度獐牙菜中?酮类成分的超高效液相色谱-电喷雾四极杆飞行时间质谱(UPLC-ESI-Q-TOF-MS)定性分析方法。方法 选用Acquity HSS T3色谱柱(100 mm×2.1 mm,1.8 μm),0.1%甲酸水-0.1%甲酸乙腈溶液作为流动相进行梯度洗脱,流速0.4 mL/min,柱温40 ℃。在正/负离子模式下采集印度獐牙菜醇提物的质谱数据,采用Masslynx4.1软件并结合SciFinder数据库、质谱数据、对照品信息和獐牙菜属植物相关文献进行数据分析。结果 在印度獐牙菜中共鉴定出?酮类化合物25个,其中3个成分为首次从印度獐牙菜中发现,分别是7-O-β-D-吡喃木糖-1, 8-二羟基-3-甲氧基?酮、Swerpunilactone B和8-O-[β-D-吡喃木糖-(1→6)-β-D-吡喃葡萄糖]-1, 7-二羟基-3-甲氧基?酮。结论 研究为印度獐牙菜中?酮类化学成分的定性分析及药材质量的控制提供实验依据。
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关键词:
- 印度獐牙菜 /
- ?酮 /
- UPLC-ESI-Q-TOF-MS
Abstract: OBJECTIVE To establish a qualitative analysis method of xanthones in Swertia chirayita by ultra-high performance liquid chromatography-time-of-flight mass spectrometry (UPLC-ESI-Q-TOF-MS).METHODS Acquity HSS T3 column (100 mm×2.1 mm, 1.8 μm) was used as the chromatographic column, with 0.1% formic acid in water-0.1% formic acid in acetonitrile as the mobile phase for gradient elution.The volume flow rate was 0.4 mL·min-1 and the column temperature was 40 ℃.In the positive and negative ion modes, the mass spectrum data of Swertia chirayita was collected and identified by Masslynx4.1 software combined with SciFinder database, comparison with mass spectrometry data analysis, reference materials and reference to relevant literatures.RESULTS A total of 25 xanthone compounds were identified, 3 of which were first discovered including 7-O-β-D-xylopyranosyl-1, 8-dihydroxy-3-methoxyxanthone, swerpunilactone B and 8-O-[β-D-xylopyranose(1→6)-β-D-glucopyranose]-1, 7-dihydroxy-3-methoxyxanthone.CONCLUSION The method can provide an experimental basis for the qualitative analysis of xanthones and the quality control of medicinal materials in Swertia chirayita.-
Key words:
- Swertia chirayita /
- xanthone /
- UPLC-ESI-Q-TOF-MS
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表 1 印度獐牙菜??酮类化合物的解谱结果
峰号 tR/min 离子模式 分子式 [M+H]+或[M-H]- 误差/10-6 离子碎片 推测成分 参考文献 实测值 理论值 1 3.205 + C19H18O11 423.093 0 423.092 7 0.7 405.082 4,387.071 1,259.024 0 芒果苷 [9] 2 3.532 - C19H18O11 421.077 1 421.077 1 0 259.023 6 异芒果苷 [10] 3 3.551 + C13H8O6 261.039 6 261.039 9 -1.1 233.043 6,215.033 8,187.044 1 ?酮(4个-OH) [11] 4* 3.623 - C19H18O10 405.081 9 405.082 2 -0.7 273.051 0 7-O-β-D-吡喃木糖-1, 8- 二羟基-3-甲氧基?酮 [12] 5 4.331 - C19H18O11 421.076 3 421.077 1 -1.9 259.024 5 ?酮(芒果苷同分异构体) [9] 6 4.512 + C13H8O4 229.050 0 229.050 1 -0.4 211.037 6,183.044 6,155.044 9 ?酮(2个-OH) [10] 7 4.664 - C13H8O4 227.034 9 227.034 4 2.2 245.045 7,183.045 5 ?酮(2个-OH) [9] 8* 4.956 - C25H28O15 567.134 0 567.135 0 -1.8 273.039 1 8-O-[β-D-吡喃木糖-(1→ 6)-β-D-吡喃葡萄糖]-1, 7- 二羟基-3-甲氧基?酮 [10, 12] 9 5.619 + C13H8O6 261.039 9 261.039 9 0 243.028 8,231.028 4,215.032 2 ?酮(4个-OH) [11] 10* 5.725 - C23H18O10 453.082 3 453.082 2 0.2 409.092 3,365.101 5,259.022 1 Swerpunilactone B [13] 11 5.935 + C13H8O6 261.039 9 261.039 9 0 243.028 9,233.043 0,215.034 0 1, 3, 5, 8-四羟基?酮 [11] 12 6.549 - C24H20O10 467.097 5 467.097 8 -0.6 423.107 2,379.118 3,349.078 2 Swerpunilactone A [13] 13 6.621 - C14H10O6 273.040 3 273.039 9 1.5 258.016 5 ?酮(3个-OH, 1个-OCH3) [14] 14 6.840 - C14H10O6 273.040 3 273.039 9 1.5 258.016 3 ?酮(3个-OH, 1个-OCH3) [14] 15 6.862 + C16H14O6 303.087 4 303.086 9 1.6 325.069 2,273.039 6,245.045 0 ?酮(1个-OH, 3个-OCH3) [15] 16 6.925 + C17H16O9 387.068 7 387.069 2 -1.3 387.068 7 ?酮(3个-OH, 4个-OCH3) [15] 17 6.975 - C14H10O6 273.040 7 273.039 9 2.9 258.016 6 ?酮(3个-OH, 1个-OCH3) [11] 18 6.989 + C14H10O6 275.055 4 275.055 6 -0.7 247.058 5 1, 5, 8-三羟基-3-甲氧基?酮 [9] 19 7.116 + C14H10O6 275.055 8 275.055 6 0.7 229.049 3,201.050 0 ?酮(3个-OH, 1个-OCH3) [11] 20 7.399 + C17H16O7 333.097 9 333.097 4 1.5 355.079 3,303.050 9,275.054 3 ?酮(1个-OH, 4个-OCH3) [16] 21 7.663 + C16H14O6 303.087 4 303.086 9 1.6 325.069 1,288.063 0,273.039 7 1-羟基-3, 7, 8-三甲氧基?酮 [17] 22 7.863 + C15H12O5 273.076 3 273.076 3 0 325.069 1,288.063 0,273.039 7 1-羟基-3, 5-二甲氧基?酮 [16] 23 8.127 + C15H12O6 289.071 4 289.071 2 0.7 245.043 1,229.050 0,215.033 7 1, 8-二羟基-3, 7-二甲氧基?酮 [17] 24 8.211 + C15H12O6 289.071 2 289.071 2 0 273.039 5,245.045 0,231.028 6 1, 8-二羟基-3, 5-二甲氧基?酮 [17] 25 8.337 + C15H12O5 273.075 8 273.076 3 -1.8 273.039 1,245.044 4,227.033 7 ?酮(1个-OH, 2个-OCH3) [16] 注:*为首次从印度獐牙菜中发现。 -
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