毛细管电泳-质谱联用法测定灵芝药材中核苷类成分
Determination of nucleosides and related compounds in Ganoderma by CE-MS
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摘要: 建立一种用于测定赤芝和紫芝中的核苷类成分的毛细管电泳-质谱联用法(CE-MS)。CE条件为：熔融石英毛细管柱(120 cm×50 μm)，缓冲液体系100 mmol/L甲酸-10%甲醇水溶液。运行电压25 kV；毛细管温度25 ℃。MS条件为：0.3%甲酸-75%甲醇水溶液为鞘液，流速3 μL/min；干燥气体流速6 L/min，干燥温度350 ℃；采用电喷雾离子化源(ESI)，正离子模式检测，全扫描范围m/z 50～350。以5-氯胞嘧啶阿拉伯糖苷为内标物。结果表明,胞嘧啶、鸟嘌呤、胞苷、腺苷、次黄嘌呤、鸟苷、肌苷和尿嘧啶在线性范围内具有较好的线性关系(除鸟苷外，其他成分R2>0.990)。加样回收率在95.3%～104.6%之间。各待测化合物的最低检测限(LOD)和最低定量限(LOQ)分别分布在0.13～9.85 μg/mL和0.42～20.83 μg/mL之间。测定结果显示赤芝的核苷类成分的含量上高于紫芝。CE-MS适合用于中药中核苷类成分的分析检测。
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关键词:
- 毛细管电泳-质谱联用法 /
- 核苷 /
- 灵芝 /
- 含量测定
Abstract: A capillary electrophoresis- mass spectrometry (CE-MS) method was established for the analysis of nucleosides and related compounds in Ganoderma lucidum and G.sinense.The separation was performed in a fused silica capillary (120 cm×50 μm) at 25 °C,with 10% methanol in water containing 100 mmol/L formic acid as CE electrolyte,and 25 kV as the applied voltage were used for the separation.The optimum MS parameters were as follows:75% methanol containing 0.3% formic acid with a flow rate of 3 μL/min was selected as the sheath liquid;the flow rate and temperature of drying gas were 6 L/min and 350 °C,respectively.ESI-MS analysis was performed in the positive mode,and the full scanning range was from m/z 50 to 350.5-Chlorocytosine arabinoside was used as the internal standard.The results showed that eight investigated compounds had good linearity (R2>0.990,except guanosine) over the tested ranges.The average recoveries were between 95.3% and 104.6%.The limit of detection (LOD) and limit of quantitation (LOQ) were 0.13-9.85 μg/mL and 0.42-20.83 μg/mL,respectively.The quantification results showed that the G.lucidum contained higher total amount of nucleosides than G.sinensis.The developed CE-MS method can be applied for the analysis of nucleosides and related compounds in Ganoderma and other traditional Chinese medicines.-
Keywords:
- CE-MS /
- nucleosides /
- Ganoderma /
- determination of content
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