柱前衍生化-高效液相色谱法同时测定含油脂药材中8种低分子羰基化合物

Simultaneous Determination of Low-molecular-weight Carbonyl Compounds in Oil-containing Herbs by HPLC Coupled with Pro-column Derivatization

目的建立高效液相色谱法（HPLC）测定含油脂类药材中低分子羰基化合物的方法。方法苦杏仁等药材经水提取，在酸性条件下，经2，4-二硝基苯肼（DNPH）衍生后，衍生物直接用HPLC测定。色谱柱：Kromasil KR100—5C18（250mm×4．6mm，5μm）；流动相：A为水-乙腈-四氢呋南-异丙醇（59：30：10：1），B为水-乙腈（35：65），梯度洗脱；流速：0．8mL／min；检测波长：365nm；柱温：30℃。结果甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮、丁醛的DNPH衍生物在-定浓度范围内与峰面积线性关系良好，相关系数均达到0．999以上，平均回收率为88．49％～93．65％，最低检测限为0．002～0．008μg／mL。结论该方法简便、灵敏、准确、重复性较好。

Objective To establish an HPLC method for determination of low-molecular-weight carbonyl compounds in the off-containing herbs. Methods After carbonyl compounds in the samples were extracted with water, the solution reacted with 2, 4-dinitrophenylhydrazine （DNPH） in an acidic medium to form 2, 4-dinitrophenylhydrazone derivatives, which were separated on Kromasil KR100-5 C18 column （250 mm × 4.6 mm, 5 μm）. The mobile phase A was water-acetonitrile-tetrahydroflaran-isopropanol （59 ： 30 ： 10 ： 1）, mobile phase B was water-acetonitrile （35 ： 65）, gradient elution. The flow rate was 0.8 mL/min, detection wavelength was 365 nm, and column temperature was 30 ℃. Results Good linearities were obtained in corresponding concentration ranges, with correlation coefficient over 0.999. The limits of detection of the eight DNPH derivatives were 0.002-0.008 μg/mL, and the average recoveries were 88.49%-93.65%. Conclusion The method is simple, accurate and reliable, with good reproducibility.