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大孔树脂SPE-RP-HPLC检测大枣中的cAMP

Determination of cAMP in Ziziphus Jujuba by Macro Porous Resins SPE - RP-HPLC

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【作者】 徐涛潘见袁传勋金日生开桂青

【Author】 XU Tao,PAN Jian,YUAN Chuan-xun,JIN Ri-sheng,KAI Gui-qing (Key Laboratory of Bioprocess of the Ministry of National Education, Hefei University of Technology, Hefei 230009, China)

【机构】 合肥工业大学农产品生物化工教育部重点实验室合肥工业大学农产品生物化工教育部重点实验室 安徽合肥230069安徽合肥230069

【摘要】 目的:建立测定大枣中环磷酸腺苷成分的反相高效液相色谱方法。方法:市售大枣切碎用20%乙醇水提取,pH与有机溶剂协同作用下经过大孔树脂梯度分离纯化环磷酸腺苷。采用WatersXterraRP18色谱柱(150mm×3.9mm,5μm);流动相为甲醇-(0.050mol/L磷酸二氢钠溶液)(10:90)系统;柱温为(30±1)℃;流速为1.0ml/min;检测波长为254nm。结果:环磷酸腺苷与其它组分的色谱峰得到基线分离。环磷酸腺苷的线性范围在0.08~0.8μg之间,相关系数r=0.9999。加样平均回收率为100.04%,环磷酸腺苷的相对标准偏差为1.21%(n=6)。最低检测限为0.5ng。结论:本方法分离效果好,快捷准确,灵敏度高,重复性好,可作为评价大枣及其制品的参考依据。

【Abstract】 Objective:To develop a method for determination of cAMP in Ziziphus Jujuba by RP-HPLC. Method: Ziziphus Jujuba was cut up and extracted by 20% ethanol -water solution. The concentrated solution was purified by micro porous resins, with elution of pH and solvent gradient. The resultant extracts were separated on a Waters Xterra RP18 column (150mm× 3.9mm,5μm) and a mobile phase of methanol-0.050molL KH2PO4 (10:90) at a flow rate of 1.0mlmin and temperature (30 ±1)℃. The detection wavelength was 254nm. Results :In the chromatogram, cAMP was separated in baseline from other ingredient. cAMP had good linearity in the range of 0.08μ g to 0.8μ g with the correlation coefficients of 0.9999. The average recovery was 100.04% with RSD 1.21%(n=6). The method permitted detection limits was as low as 0.5 ng at a signal-to-noise ratio of 3. Conclusion: The method was swift, accurate, highly sensitive and good in repetition.

【基金】 国家自然科学基金资助项目(20136020)
  • 【分类号】R284
  • 【被引频次】19
  • 【下载频次】397
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