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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
【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.
【Key words】 cAMP; micro porous resins; purification; determination; HPLC;
- 【文献出处】 食品科学 ,Food Science , 编辑部邮箱 ,2005年12期
- 【分类号】R284
- 【被引频次】19
- 【下载频次】397