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目的:建立益智中oxyphyllenodiol A(1)和teuhetenone A(2)的HPLC含量测定方法,同时对市售药材、饮片及药材不同部位中2种成分的含量进行比较研究。方法:采用高效液相色谱法,使用Waters sunfire C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-水为流动相进行梯度洗脱,流速为1.0 mL.min-1,检测波长250 nm。结果:1和2分别在0.129 6～0.864 0μg和0.163 5～1.090 0μg线性关系良好,平均回收率分别为99.08%和97.80%,在所测的不同样品中质量分数分别为0.005 9%～0.014 9%和0.008 0%～0.016 4%。1和2在益智全果中的质量分数均值分别为0.008 5%和0.010 4%;在益智种子中的质量分数均值分别为0.013 7%和0.015 7%;果壳中未检测到2种成分。结论:该方法精密、准确、重现性好,可用于测定益智药材中oxyphyllenodiol A和teuhetenone A的含量;益智全果中2种成分含量主要源于益智的种子,且在不同样品间有一定差异;盐炙益智种子和生益智种子中2种成分含量较高且无明显差异。
OBJECTIVE: To establish a HPLC method for the determination of oxyphyllenodiol A (1) and teuhetenone A (2) in the puzzle, and to compare the contents of two components in different parts of medicinal herbs, Pieces and medicinal materials. Methods: The gradient elution was performed on a Waters sunfire C18 column (4.6 mm × 250 mm, 5 μm) using acetonitrile-water as the mobile phase at a flow rate of 1.0 mL · min-1 with a detection wavelength of 250 nm . Results: The linear relationship between 1 and 2 were 0.129 6 ~ 0.864 0μg and 0.163 5 ~ 1.090 0μg respectively. The average recoveries were 99.08% and 97.80% respectively. The mass fractions of different samples were 0.005 9% ~ 0.014 9 % And 0.008 0% to 0.016 4%. The average mass fractions of 1 and 2 in the whole puzzle were 0.008 5% and 0.010 4%, respectively. The mean mass fractions in the seeds were 0.013 7% and 0.015 7% ingredient. Conclusion: The method is accurate, accurate and reproducible. It can be used to determine the content of oxyphyllenodiol A and teuhetenone A in the medicinal herbs. The content of the two components in the whole fruit is mainly derived from the seeds of Puchi, There is a certain difference; Salt Sunburn Puzzle seeds and Health Pui seeds in the two components were higher and no significant difference.