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

摘要

Objective To establish an HPLC method for determination of low-molecular-weight carbonyl compounds in the oil-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-tetrahydrofuran-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.%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 KR100-5 C18(250 mm×4.6 mm,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：0.8 mL/min；检测波长：365 nm；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衍生物在一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。