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毛细管电泳-质谱联用法测定灵芝药材中核苷类成分

杨丰庆, 张雪梅, 葛莉亚, 陈瑞银

杨丰庆, 张雪梅, 葛莉亚, 陈瑞银. 毛细管电泳-质谱联用法测定灵芝药材中核苷类成分[J]. 中国药科大学学报, 2011, 42(4): 337-341.
引用本文: 杨丰庆, 张雪梅, 葛莉亚, 陈瑞银. 毛细管电泳-质谱联用法测定灵芝药材中核苷类成分[J]. 中国药科大学学报, 2011, 42(4): 337-341.
YANG Feng-qing, ZHANG Xue-mei, GE Li-ya, TAN Swee Ngin. Determination of nucleosides and related compounds in Ganoderma by CE-MS[J]. Journal of China Pharmaceutical University, 2011, 42(4): 337-341.
Citation: YANG Feng-qing, ZHANG Xue-mei, GE Li-ya, TAN Swee Ngin. Determination of nucleosides and related compounds in Ganoderma by CE-MS[J]. Journal of China Pharmaceutical University, 2011, 42(4): 337-341.

毛细管电泳-质谱联用法测定灵芝药材中核苷类成分

基金项目: 重庆市科委自然科学基金资助项目(No.2010BB5070);重庆大学211工程三期创新人才培养计划建设项目资助(No.S-09103)

Determination of nucleosides and related compounds in Ganoderma by CE-MS

  • 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。
    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.
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  • 刊出日期:  2011-08-24

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