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目的:应用超声-微波协同萃取技术提取金线莲中的腺嘌呤,高效液相色谱法-电喷雾电离/离子阱质谱法(HPLC-ESI/MS)对提取物中腺嘌呤进行测定和鉴别。方法:色谱条件为Agilent TC-C18色谱柱(5μm,4.6mm×250mm),流动相为甲醇∶0.02mol.L-1醋酸-醋酸铵缓冲溶液(5∶95,pH 4.6),流速1.0mL.min-1,检测波长260nm,柱温:30℃。结果:表明腺嘌呤浓度在0.5～60.0μg.mL-1范围内呈良好线性关系,相关系数为0.999 9,回收率在95.4%～96.2%之间,相对标准偏差为0.45%,测得金线莲(产于广西)提取物中腺嘌呤含量为10.64μg.g-1,结论:该法方法操作简便,灵敏快速。迄今为止,首次报道金线莲中含有重要药理活性的物质腺嘌呤,为金线莲的药理和临床试验研究提供物质基础。
OBJECTIVE: To extract adenine from A. chinense by ultrasonic-microwave co-extraction and determine and identify adenine by HPLC-ESI / MS. Methods: The chromatographic conditions were Agilent TC-C18 column (5μm, 4.6mm × 250mm) and mobile phase consisted of methanol: 0.02mol·L-1 acetic acid-ammonium acetate buffer solution (5:95, pH 4.6) at a flow rate of 1.0mL. min-1, detection wavelength 260nm, column temperature: 30 ℃. The results showed that the concentration of adenine showed a good linearity in the range of 0.5-60.0μg.mL-1, the correlation coefficient was 0.999 9, the recovery was between 95.4% -96.2% and the relative standard deviation was 0.45% Lin (produced in Guangxi) extract adenine content of 10.64μg.g-1, Conclusion: The method is simple, fast and sensitive. Up to now, adenine, a substance containing important pharmacological activity, has been reported for the first time, providing the material basis for the pharmacological and clinical trials of A. sinense.